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Sample records for acidity soluble solids

  1. 7 CFR 51.1178 - Maximum anhydrous citric acid permissible for corresponding total soluble solids.

    Code of Federal Regulations, 2013 CFR

    2013-01-01

    ... corresponding total soluble solids. 51.1178 Section 51.1178 Agriculture Regulations of the Department of... corresponding total soluble solids. For determining the grade of juice, the maximum permissible anhydrous citric acid content in relation to corresponding total soluble solids in the fruit is set forth in...

  2. 7 CFR 51.1178 - Maximum anhydrous citric acid permissible for corresponding total soluble solids.

    Code of Federal Regulations, 2014 CFR

    2014-01-01

    ... corresponding total soluble solids. 51.1178 Section 51.1178 Agriculture Regulations of the Department of... corresponding total soluble solids. For determining the grade of juice, the maximum permissible anhydrous citric acid content in relation to corresponding total soluble solids in the fruit is set forth in...

  3. 7 CFR 51.1178 - Maximum anhydrous citric acid permissible for corresponding total soluble solids.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ... corresponding total soluble solids. 51.1178 Section 51.1178 Agriculture Regulations of the Department of... solids. For determining the grade of juice, the maximum permissible anhydrous citric acid content in relation to corresponding total soluble solids in the fruit is set forth in the following Table II...

  4. 7 CFR 51.1178 - Maximum anhydrous citric acid permissible for corresponding total soluble solids.

    Code of Federal Regulations, 2011 CFR

    2011-01-01

    ... corresponding total soluble solids. 51.1178 Section 51.1178 Agriculture Regulations of the Department of... solids. For determining the grade of juice, the maximum permissible anhydrous citric acid content in relation to corresponding total soluble solids in the fruit is set forth in the following Table II...

  5. 7 CFR 51.1178 - Maximum anhydrous citric acid permissible for corresponding total soluble solids.

    Code of Federal Regulations, 2012 CFR

    2012-01-01

    ... corresponding total soluble solids. 51.1178 Section 51.1178 Agriculture Regulations of the Department of... solids. For determining the grade of juice, the maximum permissible anhydrous citric acid content in relation to corresponding total soluble solids in the fruit is set forth in the following Table II...

  6. Relationship of soluble solids, acidity and aroma volatiles to flavor in late-season navel oranges

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Navel orange flavor development during early fruit maturation is strongly dependent on changes in soluble solids concentration (SSC) and titratable acidity (TA), while later in the season other factors, such as aroma volatiles, also become important. The flavor of individual oranges can differ gre...

  7. Stability and solubility enhancement of ellagic acid in cellulose ester solid dispersions.

    PubMed

    Li, Bin; Harich, Kim; Wegiel, Lindsay; Taylor, Lynne S; Edgar, Kevin J

    2013-02-15

    Structurally varied, carboxyl-containing cellulose derivatives were evaluated for their ability to form amorphous solid dispersions (ASD) with ellagic acid (EA), in order to improve the solubility of this high-melting, poorly bioavailable, but highly bioactive natural flavonoid compound. ASDs of EA with carboxymethylcellulose acetate butyrate (CMCAB), cellulose acetate adipate propionate (CAAdP), and hydroxypropylmethylcellulose acetate succinate (HPMCAS) were prepared, and EA dissolution from these ASDs was compared with that from pure crystalline EA and from EA/poly(vinylpyrrolidinone) (PVP) solid dispersions (SD). Polymer/drug mixtures were characterized by powder X-ray diffraction (XRPD), modulated differential scanning calorimetry (MDSC), nuclear magnetic resonance (NMR) and Fourier transform infrared spectroscopy (FT-IR). The XRPD and FT-IR results indicated that EA was amorphous in solid dispersions with EA concentration up to 25 wt%. The stability against crystallization and solution concentrations of EA from these solid dispersions were significantly higher than those observed for physical mixtures and pure crystalline EA. HPMCAS stabilized EA most effectively, among the polymers tested, against both chemical degradation and recrystallization. The relative ability to solubilize EA from ASDs at pH 6.8 was PVP>HPMCAS>CMCAB. EA dissolves from ASD in PVP quickly and completely (maximum 92%) at pH 6.8, but EA is also released from PVP at pH 1.2, and then crystallizes rapidly. Therefore PVP is not a practical candidate for EA ASD. In contrast, the cellulose derivative ASDs show very slow EA release at pH 1.2 (<4%) and faster but still incomplete drug release at pH 6.8 (maximum 35% for HPMCAS SD). The pH-triggered drug release from HPMCAS ASD makes HPMCAS a practical choice for EA solubility enhancement. PMID:23399175

  8. Cryomilling-induced solid dispersion of poor glass forming/poorly water-soluble mefenamic acid with polyvinylpyrrolidone K12.

    PubMed

    Kang, Naewon; Lee, Jangmi; Choi, Ji Na; Mao, Chen; Lee, Eun Hee

    2015-06-01

    The effect of mechanical impact on the polymorphic transformation of mefenamic acid (MFA) and the formation of a solid dispersion of mefenamic acid, a poor glass forming/poorly-water soluble compound, with polyvinylpyrrolidone (PVP) K12 was investigated. The implication of solid dispersion formation on solubility enhancement of MFA, prepared by cryomilling, was investigated. Solid state characterization was conducted using powder X-ray diffraction (PXRD) and Fourier-transform infrared (FTIR) spectroscopy combined with crystal structure analysis. Apparent solubility of the mixtures in pH 7.4 buffer was measured. A calculation to compare the powder patterns and FTIR spectra of solid dispersions with the corresponding physical mixtures was conducted. Solid state characterization showed that (1) MFA I transformed to MFA II when pure MFA I was cryogenically milled (CM); and (2) MFA forms a solid dispersion when MFA was cryogenically milled with PVP K12. FTIR spectral analysis showed that hydrogen bonding facilitated by mechanical impact played a major role in forming solid dispersions. The apparent solubility of MFA was significantly improved by making a solid dispersion with PVP K12 via cryomilling. This study highlights the importance of cryomilling with a good hydrogen bond forming excipient as a technique to prepare solid dispersion, especially when a compound shows a poor glass forming ability and therefore, is not easy to form amorphous forms by conventional method. PMID:24849785

  9. A comparison of the use of BrimA versus soluble solids/titratable acidity ratio as a maturity standard for navel oranges

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Maturity and time of harvest for California navel oranges is primarily determined by the ratio of the soluble solids concentration (SSC) to titratable acidity (TA). This standard has been used in the industry for decades but its usefulness and relationship to flavor have often been questioned. In re...

  10. Determination of soluble solids content and titratable acidity of intact fruit and juice of Satsuma mandarin using a hand-held NIR instrument in transmittance mode

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Determination of soluble solids content (SSC) and titratable acidity (TA) of intact fruit and juice of Satsuma mandarin was investigated using a hand-held NIR instrument “NIR-Gun” in transmittance mode. The resulting calibration equation measured SSC of intact fruit and juice with a standard error o...

  11. Production of a water-soluble fertilizer containing amino acids by solid-state fermentation of soybean meal and evaluation of its efficacy on the rapeseed growth.

    PubMed

    Wang, Jianlei; Liu, Zhemin; Wang, Yue; Cheng, Wen; Mou, Haijin

    2014-10-10

    Soybean meal is a by-product of soybean oil extraction and contains approximately 44% protein. We performed solid-state fermentation by using Bacillus subtilis strain N-2 to produce a water-soluble fertilizer containing amino acids. Strain N-2 produced a high yield of protease, which transformed the proteins in soybean meal into peptide and free amino acids that were dissolved in the fermentation products. Based on the Plackett-Burman design, the initial pH of the fermentation substrate, number of days of fermentation, and the ratio of liquid to soybean meal exhibited significant effects on the recovery of proteins in the resulting water-soluble solution. According to the predicted results of the central composite design, the highest recovery of soluble proteins (99.072%) was achieved at the optimum conditions. Under these conditions, the resulting solution contained 50.42% small peptides and 7.9% poly-γ-glutamic acid (γ-PGA). The water-soluble fertilizer robustly increased the activity of the rapeseed root system, chlorophyll content, leaf area, shoot dry weight, root length, and root weight at a concentration of 0.25% (w/v). This methodology offers a value-added use of soybean meal. PMID:25062659

  12. Solid inclusion complexes of oleanolic acid with amino-appended β-cyclodextrins (ACDs): Preparation, characterization, water solubility and anticancer activity.

    PubMed

    Ren, Yufeng; Liu, Ying; Yang, Zhikuan; Niu, Raomei; Gao, Kai; Yang, Bo; Liao, Xiali; Zhang, Jihong

    2016-12-01

    Oleanolic acid (OA) is a pentacyclic triterpenoid acid of natural abundance in plants which possesses important biological activities. However, its medicinal applications were severely impeded by the poor water solubility and resultant low bioavailability and potency. In this work, studies on solid inclusion complexes of OA with a series of amino-appended β-cyclodextrins (ACDs) were conducted in order to address this issue. These complexes were prepared by suspension method and were well characterized by NMR, SEM, XRD, TG, DSC and Zeta potential measurement. The 2:1 inclusion mode of ACDs/OA complexes was elucidated by elaborate 2D NMR (ROESY). Besides, water solubility of OA was dramatically promoted by inclusion complexation with ACDs. Moreover, in vitro anticancer activities of OA against human cancer cell lines HepG2, HT29 and HCT116 were significantly enhanced after formation of inclusion complexes, while the apoptotic response results indicated their induction of apoptosis of cancer cells. This could provide a novel approach to development of novel pharmaceutical formulations of OA. PMID:27612690

  13. Nondestructive quantification of the soluble-solids content and the available acidity of apples by Fourier-transform near-infrared spectroscopy

    SciTech Connect

    Ying Yibin; Liu Yande; Tao Yang

    2005-09-01

    This research evaluated the feasibility of using Fourier-transform near-infrared (FT-NIR) spectroscopy to quantify the soluble-solids content (SSC) and the available acidity (VA) in intact apples. Partial least-squares calibration models, obtained from several preprocessing techniques (smoothing, derivative, etc.) in several wave-number ranges were compared. The best models were obtained with the high coefficient determination (r{sup 2}) 0.940 for the SSC and a moderate r{sup 2} of 0.801 for the VA, root-mean-square errors of prediction of 0.272% and 0.053%, and root-mean-square errors of calibration of 0.261% and 0.046%, respectively. The results indicate that the FT-NIR spectroscopy yields good predictions of the SSC and also showed the feasibility of using it to predict the VA of apples.

  14. AN-107 entrained solids - Solubility versus temperature

    SciTech Connect

    GJ Lumetta; RC Lettau

    2000-03-31

    This report describes the results of a test conducted by Battelle to assess the solubility of the solids entrained in the diluted AN-107 low-activity waste (LAW) sample. BNFL requested Battelle to dilute the AN-107 sample using sodium hydroxide and de-ionized water to mimic expected plant operating conditions. BNFL further requested Battelle to assess the solubility of the solids present in the diluted AN-107 sample versus temperature conditions of 30, 40, and 50 C. BNFL requested these tests to assess the composition of the LAW supernatant and solids versus expected plant-operating conditions.

  15. AW-101 entrained solids - Solubility versus temperature

    SciTech Connect

    GJ Lumetta; RC Lettau; GF Piepel

    2000-03-31

    This report describes the results of a test conducted by Battelle to assess the solubility of the solids entrained in the diluted AW-101 low-activity waste (LAW) sample. BNFL requested Battelle to dilute the AW-1-1 sample using de-ionized water to mimic expected plant operating conditions. BNFL further requested Battelle to assess the solubility of the solids present in the diluted AW-101 sample versus temperature conditions of 30, 40, and 50 C. BNFL requested these tests to assess the composition of the LAW supernatant and solids versus expected plant-operating conditions. The work was conducted according to test plan BNFL-TP-29953-7, Rev. 0, Determination of the Solubility of LAW Entrained Solids. The test went according to plan, with no deviations from the test plan.

  16. Production of furfural from xylose, water-insoluble hemicelluloses and water-soluble fraction of corncob via a tin-loaded montmorillonite solid acid catalyst.

    PubMed

    Li, Huiling; Ren, Junli; Zhong, Linjie; Sun, Runcang; Liang, Lei

    2015-01-01

    The conversion of xylose, water-insoluble hemicelluloses (WIH) and water-soluble fraction (WSF) of corncob to furfural was performed using montmorillonite with tin ions (Sn-MMT) containing double acid sites as a solid acid catalyst. The co-existence of Lewis acids and Brønsted acids in Sn-MMT was shown to improve the furfural yield and selectivity. 76.79% furfural yield and 82.45% furfural selectivity were obtained from xylose using Sn-MMT as a catalyst in a biphasic system with 2-s-butylphenol (SBP) as the organic extracting layer and dimethyl sulfoxide (DMSO) as the co-solvent in contact with an aqueous phase saturated with NaCl (SBP/NaCl-DMSO) at 180°C for 30min. Furthermore, Sn-MMT also demonstrated the excellent catalytic performance in the conversion of pentose-rich materials of corncob and 39.56% and 54.15% furfural yields can be directly obtained from WIH and WSF in the SBP/NaCl-DMSO system, respectively. PMID:25461009

  17. Acid soluble, pepsin resistant platelet aggregating material

    SciTech Connect

    Schneider, M.D.

    1982-08-31

    Disclosed is an acid soluble, pepsin resistant, platelet aggregating material isolated from equine arterial tissue by extraction with dilute aqueous acid. The method of isolation and use to control bleeding are described. 4 figs.

  18. Factors affecting ethylene and carbon dioxide concentrations during ripening: Incidence on final dry matter, total soluble solids content and acidity of mango fruit.

    PubMed

    Nordey, Thibault; Léchaudel, Mathieu; Génard, Michel; Joas, Jacques

    2016-06-01

    Ripening of climacteric fruits is associated with pronounced changes in fruit gas composition caused by a concomitant rise in respiration and ethylene production. There is a discrepancy in the literature since some authors reported that changes in fruit gas compositions differ in attached and detached fruits. This study presents for the first time an overview of pre- and post-harvest factors that lead to variations in the climacteric respiration and ethylene production, and attempts to determine their impacts on fruit composition, i.e., dry matter, total soluble solids content and acidity. The impact of growing conditions such as the fruit position in the canopy and the fruit carbon supply; fruit detachment from the tree, including the maturity stage at harvest; and storage conditions after harvest, i.e., relative humidity and temperature were considered as well as changes in fruit skin resistance to gas diffusion during fruit growth and storage. Results showed that fruit gas composition vary with all pre and post-harvest factors studied. Although all mangoes underwent a respiratory climacteric and an autocatalytic ethylene production, whatever pre and post-harvest factors studied, large differences in ethylene production, climacteric respiration and fruit quality were measured. Results suggested that the ripening capacity is not related to the fruit ability to produce great amount of ethylene. In agreement with precedent studies, this work provided several lines of evidence that gas composition of fruit is related to its water balance. Our measurements indicated that skin resistance to gas diffusion increased after the harvest and during storage. It was so suggested that the faster ripening of detached fruit may be explained in part by changes in fruit water balance and skin resistance to gas diffusion caused by fruit detachment. PMID:27085177

  19. Transformation of acidic poorly water soluble drugs into ionic liquids.

    PubMed

    Balk, Anja; Wiest, Johannes; Widmer, Toni; Galli, Bruno; Holzgrabe, Ulrike; Meinel, Lorenz

    2015-08-01

    Poor water solubility of active pharmaceutical ingredients (API) is a major challenge in drug development impairing bioavailability and therapeutic benefit. This study is addressing the possibility to tailor pharmaceutical and physical properties of APIs by transforming these into tetrabutylphosphonium (TBP) salts, including the generation of ionic liquids (IL). Therefore, poorly water soluble acidic APIs (Diclofenac, Ibuprofen, Ketoprofen, Naproxen, Sulfadiazine, Sulfamethoxazole, and Tolbutamide) were converted into TBP ILs or low melting salts and compared to the corresponding sodium salts. Free acids and TBP salts were characterized by NMR and IR spectroscopy, DSC and XRPD, DVS and dissolution rate measurements, release profiles, and saturation concentration measurements. TBP salts had lower melting points and glass transition temperatures and dissolution rates were improved up to a factor of 1000 as compared to the corresponding free acid. An increase in dissolution rates was at the expense of increased hygroscopicity. In conclusion, the creation of TBP ionic liquids or solid salts from APIs is a valuable concept addressing dissolution and solubility challenges of poorly water soluble acidic compounds. The data suggested that tailor-made counterions may substantially expand the formulation scientist's armamentarium to meet challenges of poorly water soluble drugs. PMID:25976317

  20. Improvement in solubility of poor water-soluble drugs by solid dispersion

    PubMed Central

    Sareen, Swati; Mathew, George; Joseph, Lincy

    2012-01-01

    This article is intended to combine recent literature on solid dispersion technology for solubility enhancement with special emphasis on mechanism responsible for the same by solid dispersion, various preparation methods, and evaluation parameters. Solubility behavior is the most challenging aspect for various new chemical entities as 60% of the new potential products possess solubility problems. This is the biggest reason for new drug molecules not reaching to the market or not reaches to full potential. There are various techniques to enhance the drug solubility such as particle size reduction, nanosuspension, use of surfactants, salt formation, solid dispersion, etc. From this article it may be concluded that solid dispersion is an important approach for improvement of bioavailability of poor water-soluble drugs. PMID:23071955

  1. Ultrasound influence on the solubility of solid dispersions prepared for a poorly soluble drug.

    PubMed

    Pereira, Simone Vieira; Colombo, Fábio Belotti; de Freitas, Luis Alexandre Pedro

    2016-03-01

    Solid dispersions have been successfully used to enhance the solubility of several poorly water soluble drugs. Solid dispersions are produced by melting hydrophilic carriers and mixing in the poorly water soluble drug. Supersaturation is obtained by quickly cooling the mixture until it solidifies, thereby entrapping the drug. The effects of using ultrasound to homogenize the molten carrier and drug mixture were studied. In particular, the increase in drug solubility for the resulting solid dispersions was analyzed. Piroxicam, which has very low water solubility, was used as a model drug. A full factorial design was used to analyze how sonication parameters affected the solubility and in vitro release of the drug. The results show that the use of ultrasound can significantly increase the solubility and dissolution rate of the piroxicam solid dispersion. Pure piroxicam presented a solubility of 13.3 μg/mL. A maximum fourfold increase in solubility, reaching 53.8 μg/mL, was observed for a solid dispersion sonicated at 19 kHz for 10 min and 475 W. The in vitro dissolution rate test showed the sonicated solid dispersion reached a maximum rate of 18%/min, a sixfold increase over the piroxicam rate of 2.9%/min. Further solid state characterization by thermal, X-ray diffraction and Fourier transform infrared analyses also showed that the sonication process, in the described conditions, did not adversely alter the drug or significantly change its polymorphic form. Ultrasound is therefore an interesting technique to homogenize drug/carrier mixtures with the objective of increasing the solubility of drugs with poor water solubility. PMID:26548840

  2. Solubility of Sulfur Dioxide in Sulfuric Acid

    NASA Technical Reports Server (NTRS)

    Chang, K. K.; Compton, L. E.; Lawson, D. D.

    1982-01-01

    The solubility of sulfur dioxide in 50% (wt./wt.) sulfuric acid was evaluated by regular solution theory, and the results verified by experimental measurements in the temperature range of 25 C to 70 C at pressures of 60 to 200 PSIA. The percent (wt./wt.) of sulfur dioxide in 50% (wt./wt.) sulfuric acid is given by the equation %SO2 = 2.2350 + 0.0903P - 0.00026P 10 to the 2nd power with P in PSIA.

  3. Solubility Enhancement of a Poorly Water Soluble Drug by Forming Solid Dispersions using Mechanochemical Activation

    PubMed Central

    Rojas-Oviedo, I.; Retchkiman-Corona, B.; Quirino-Barreda, C. T.; Cárdenas, J.; Schabes-Retchkiman, P. S.

    2012-01-01

    Mechanochemical activation is a practical cogrinding operation used to obtain a solid dispersion of a poorly water soluble drug through changes in the solid state molecular aggregation of drug-carrier mixtures and the formation of noncovalent interactions (hydrogen bonds) between two crystalline solids such as a soluble carrier, lactose, and a poorly soluble drug, indomethacin, in order to improve its solubility and dissolution rate. Samples of indomethacin and a physical mixture with a weight ratio of 1:1 of indomethacin and lactose were ground using a high speed vibrating ball mill. Particle size was determined by electron microscopy, the reduction of crystallinity was determined by calorimetry and transmission electron microscopy, infrared spectroscopy was used to find evidence of any interactions between the drug and the carrier and the determination of apparent solubility allowed for the corroboration of changes in solubility. Before grinding, scanning electron microscopy showed the drug and lactose to have an average particle size of around 50 and 30 μm, respectively. After high speed grinding, indomethacin and the mixture had a reduced average particle size of around 5 and 2 μm, respectively, showing a morphological change. The ground mixture produced a solid dispersion that had a loss of crystallinity that reached 81% after 30 min of grinding while the drug solubility of indomethacin within the solid dispersion increased by 2.76 fold as compared to the pure drug. Drug activation due to hydrogen bonds between the carboxylic group of the drug and the hydroxyl group of lactose as well as the decrease in crystallinity of the solid dispersion and the reduction of the particle size led to a better water solubility of indomethacin. PMID:23798775

  4. GADOLINIUM OXALATE SOLUBILITY MEASUREMENTS IN NITRIC ACID SOLUTIONS

    SciTech Connect

    Pierce, R. A.

    2012-03-12

    HB-Line will begin processing Pu solutions during FY2012 that will involve the recovery of Pu using oxalate precipitation and filtration. After the precipitation and filtration processes, the filtrate solution will be transferred from HB-Line to H-Canyon. The presence of excess oxalate and unfiltered Pu oxalate solids in these solutions create a criticality safety issue if they are sent to H-Canyon without controls in H-Canyon. One approach involves H-Canyon receiving the filtrate solution into a tank that is poisoned with soluble gadolinium (Gd). Decomposition of the oxalate will occur within a subsequent H-Canyon vessel. The receipt of excess oxalate into the H-Canyon receipt tanks has the potential to precipitate a portion of the Gd poison in the receipt tanks. Because the amount of Gd in solution determines the maximum amount of Pu solids that H-Canyon can receive, H-Canyon Engineering requested that SRNL determine the solubility of Gd in aqueous solutions of 4-10 M nitric acid (HNO{sub 3}), 4-12 g/L Gd, and 0.15-0.25 M oxalic acid (H{sub 2}C{sub 2}O{sub 4}) at 25 °C. The target soluble Gd concentration is 6 g/L. The data indicate that the target can be achieved above 6 M HNO{sub 3} and below 0.25 M H{sub 2}C{sub 2}O{sub 4}. At 25 °C, for 6 M HNO{sub 3}, 11 g/L and 7 g/L Gd are soluble in 0.15 M and 0.25 M H{sub 2}C{sub 2}O{sub 4}, respectively. In 4 M HNO{sub 3}, the Gd solubility drops significantly to 2.5 g/L and 0.8 g/L in 0.15 M and 0.25 M H{sub 2}C{sub 2}O{sub 4}, respectively. The solubility of Gd at 8-10 M HNO{sub 3} exceeds the solubility at 6 M HNO{sub 3}. The data for 4 M HNO{sub 3} showed good agreement with data in the literature. To achieve a target of 6 g/L soluble Gd in solution in the presence of 0.15-0.25 M oxalate, the HNO{sub 3} concentration must be maintained at or above 6 M HNO{sub 3}. The solubility of Gd in 4 M HNO{sub 3} with 0.15 M oxalate at 10 °C is about 1.5 g/L. For 6 M HNO{sub 3} with 0.15 M oxalate, the solubility of Gd at 10

  5. GADOLINIUM OXALATE SOLUBILITY MEASUREMENTS IN NITRIC ACID SOLUTIONS

    SciTech Connect

    Pierce, R.

    2012-02-22

    HB-Line will begin processing Pu solutions during FY2012 that will involve the recovery of Pu using oxalate precipitation and filtration. After the precipitation and filtration processes, the filtrate solution will be transferred from HB-Line to H-Canyon. The presence of excess oxalate and unfiltered Pu oxalate solids in these solutions create a criticality safety issue if they are sent to H-Canyon without controls in H-Canyon. One approach involves H-Canyon receiving the filtrate solution into a tank that is poisoned with soluble gadolinium (Gd). Decomposition of the oxalate will occur within a subsequent H-Canyon vessel. The receipt of excess oxalate into the H-Canyon receipt tanks has the potential to precipitate a portion of the Gd poison in the receipt tanks. Because the amount of Gd in solution determines the maximum amount of Pu solids that H-Canyon can receive, H-Canyon Engineering requested that SRNL determine the solubility of Gd in aqueous solutions of 4-10 M nitric acid (HNO{sub 3}), 4-12 g/L Gd, and 0.15-0.25 M oxalic acid (H{sub 2}C{sub 2}O{sub 4}) at 25 C. The target soluble Gd concentration is 6 g/L. The data indicate that the target can be achieved above 6 M HNO{sub 3} and below 0.25 M H{sub 2}C{sub 2}O{sub 4}. For 6 M HNO{sub 3}, 10.5 g/L and 7 g/L Gd are soluble in 0.15 M and 0.25 M H{sub 2}C{sub 2}O{sub 4}, respectively. In 4 M HNO{sub 3}, the Gd solubility drops significantly to 2 g/L and 0.25 g/L in 0.15 M and 0.25 M H{sub 2}C{sub 2}O{sub 4}, respectively. The solubility of Gd at 8-10 M HNO{sub 3} exceeds the solubility at 6 M HNO{sub 3}. The data for 4 M HNO{sub 3} showed good agreement with data in the literature. To achieve a target of 6 g/L soluble Gd in solution in the presence of 0.15-0.25 M oxalate, the HNO{sub 3} concentration must be maintained at or above 6 M HNO{sub 3}.

  6. Joint solubility of samarium and dysprosium in solid magnesium

    NASA Astrophysics Data System (ADS)

    Rokhlin, L. L.; Dobatkina, T. V.; Lukyanova, E. A.; Korolkova, I. G.; Tarytina, I. E.

    2016-03-01

    The phase compositions of solid Mg-Sm-Dy alloys corresponding to the magnesium-corner region of the phase diagram are studied by optical and scanning electron microscopy, electrical resistivity measurements, and electron microprobe analysis. The obtained results allowed us to determine the joint solubility of samarium and dysprosium in solid magnesium at 500, 400, and 300°C; it decreases with decreasing temperature. The magnesium solid solution is found to be in equilibrium only with the Mg41Sm5 and Mg24Dy5 compounds, which are in equilibrium with the magnesium solid solution in the binary Mg-Sm and Mg-Dy systems.

  7. Solubility and thermodynamic properties of oxygen in solid molybdenum

    NASA Technical Reports Server (NTRS)

    Srivastava, S. C.; Seigle, L. L.

    1974-01-01

    A formula is obtained for the solubility of oxygen in solid Mo, determined in the range from 1400 to 1900 C by equilibrating rods of zone-refined Mo with mixtures of Mo and MoO2 powders. Using the known value of the free energy of formation of MoO2, a formula is obtained for the chemical potential of oxygen in the dilute solid solution. The heat of solution of oxygen in solid Mo and the excess entropy for the interstitial solid solution are also determined, assuming that the oxygen atoms reside in the octahedral interstices of bcc Mo.

  8. Effects of solids content, settling temperature, and liquor source on tall oil solubilities

    SciTech Connect

    Rousseau, R.W.; Kassebi, A.; Zinkel, D.F.

    1984-01-01

    Tall oil soap solubility in black liquors obtained from cooking pine and sweet gum, and in mixture of these liquors, was studied. As expected, solids content had a significant effect on the amount of soap remaining in settled liquors obtained from pine. Concentrating these liquors to about 30% solids reduced the soap concentration to approximately 0.8% of solids. Increasing the temperature at which the liquors were settled also increased residual tall oil soap content. Although mass balance calculations on mixtures of black liquors obtained from pine and gum show that the percentage recovery (solids basis) varies little with the inclusion of 12 to 50% hardwood black liquor, absolute recovery is increased with increased proportions of hardwood liquor. This is the result of decreased soap solubility with increased proportions of hardwood liquor. No discernable effect was observed on the proportion and composition of the acids and neutrals of the dissolved tall oil with respect to the solids content of the liquors.

  9. In vitro Dissolution Studies on Solid Dispersions of Mefenamic Acid

    PubMed Central

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

    2011-01-01

    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. PMID:22303074

  10. Solubility of strontium-substituted apatite by solid titration.

    PubMed

    Pan, H B; Li, Z Y; Lam, W M; Wong, J C; Darvell, B W; Luk, K D K; Lu, W W

    2009-06-01

    Solid titration was used to explore the solubility isotherms of partially (Srx-HAp, x=1, 5, 10, 40, 60 mol.%) and fully substituted strontium hydroxyapatite (Sr-HAp). Solubility increased with increasing strontium content. No phase other than strontium-substituted HAp, corresponding to the original titrant, was detected in the solid present at equilibrium; in particular, dicalcium hydrogen phosphate was not detected at low pH. The increase in solubility with strontium content is interpreted as a destabilization of the crystal structure by the larger strontium ion. Carbonated HAp was formed in simulated body fluid containing carbonate on seeding with Sr10-HAp, but the precipitate was strontium-substituted on seeding with Sr-HAp. Strontium-substituted HAp might be usable as a template for the growth of new bone, since nucleation appears to be facilitated. PMID:19135423

  11. Prediction of soluble solids content of blueberries using hyperspectral imaging

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Soluble solids content (SSC) is one of the most important quality parameters for blueberry, and it directly relates to the marketability and shelf life of fresh blueberries. Currently, color imaging technology is being used for color and size grading of fruits like blueberry. The technology is, howe...

  12. Influences of heating temperature, pH, and soluble solids on the decimal reduction times of acid-adapted and non-adapted Escherichia coli O157:H7 (HCIPH 96055) in a defined liquid heating medium.

    PubMed

    Gabriel, Alonzo A

    2012-11-01

    The study characterized the influences of various combinations of process and product parameters namely, heating temperature (53, 55, 57.5, 60, 62 °C), pH (2.0, 3.0, 4.5, 6.0, 7.0), and soluble solids (SS) (1.4, 15, 35, 55, 69°Brix) on the thermal inactivation of non-adapted and acid-adapted E. coli O157:H7 (HCIPH 96055) in a defined liquid heating medium (LHM). Acid adaptation was conducted by propagating cells in a gradually acidifying nutrient broth medium, supplemented with 1% glucose. The D values of non-adapted cells ranged from 1.43 s (0.02 min) to 304.89 s (5.08 min). Acid-adapted cells had D values that ranged from 1.33 s (0.02 min) to 2628.57 s (43.81 min). Adaptation did not always result in more resistant cells as indicated by the Log (D(adapted)/D(non-adapted)) values calculated in all combinations tested, with values ranging from -1.10 to 1.40. The linear effects of temperature and pH, and the joint effects of pH and SS significantly influenced the thermal resistance of non-adapted cells. Only the linear and quadratic effects of both pH and SS significantly influenced the D values of acid-adapted cells. Generally, the D values of acid-adapted cells decreased at SS greater than 55 °Brix, suggesting the possible cancelation of thermal cross protection by acid habituation at such SS levels. The relatively wide ranges of LHM pH and SS values tested in the study allowed for better examination of the effects of these factors on the thermal death of the pathogen. The results established in this work may be used in the evaluation, control and improvement of safety of juice products; and of other liquid foods with physicochemical properties that fall within the ranges tested in this work. PMID:23141645

  13. Solubility of chlorine in aqueous hydrochloric acid solutions.

    PubMed

    Alkan, Mahir; Oktay, Münir; Kocakerim, M Muhtar; Copur, Mehmet

    2005-03-17

    The solubility of chlorine in aqueous hydrochloric acid solutions was studied. The effects of HCl concentration and temperature on the solubility were evaluated, and the thermodynamic parameters of the dissolution were calculated. It was found that the solubility isotherms had a minimum at about 0.5M HCl concentration at all the temperatures studied and that solubility decreased with the increase of temperature at all the HCl concentration range investigated. PMID:15752843

  14. Acid soluble platelet aggregating material isolated from human umbilical cord

    SciTech Connect

    Schneider, M.D.

    1983-12-27

    An acid soluble, pepsin sensitive platelet aggregating material is isolated from human umbilical cord tissue by extraction with dilute aqueous acid. The method of isolation is disclosed and its use to control bleeding is described. 2 figs.

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

    PubMed

    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. PMID:23244679

  16. The solubility of aluminum in acidic forest soils: Long-term changes due to acid deposition

    NASA Astrophysics Data System (ADS)

    Mulder, Jan; Stein, Alfred

    1994-01-01

    Despite the ecological and pedogenic importance of Al, its solubility control in acidic forest soils is poorly understood. Here we discuss the solubility of Al and its development with time in three acid brown forest soils in The Netherlands, which are under extreme acidification from atmospheric deposition. All soil solutions (to a 60 cm depth) were undersaturated with respect to synthetic gibbsite (Al(OH) 3; log K = 9.12 at 8°C), with the highest degree of undersaturation occurring in the surface soil. In about one third of the individual soil layers a significant positive correlation existed between the activity of Al 3+ and H +, but this relationship was far less than cubic. Kinetically constrained dissolution of Al is unlikely to explain the disequilibrium with respect to gibbsite, because undersaturation was highest through summer when water residence times were longest and temperatures greatest. Time series analysis of six year data sets for several soil layers revealed a significant annual decline in soil solution pH and Al solubility (defined as log Al + 3 pH) despite a constant concentration of strong acid anions. The annual decline of both pH and Al solubility was greatest in the surface soil and was positively correlated with the relative depletion of reactive organically bound soil Al. The results support our earlier hypothesis that in strongly acidified forest soils complexation by solid phase organics controls the solubility of Al even in mineral soil layers, relatively low in organic C. The data lend no support to the current widespread and often uncritical use of gibbsite as a model for the Al solubility in highly acidic forest soils (pH < 4.5) of the temperate zone.

  17. Solubility series of methanofullerenes in concentrated sulfuric acid

    NASA Astrophysics Data System (ADS)

    Biglova, Yu. N.; Kolesov, S. V.; Biglova, R. Z.; Kraikin, V. A.

    2015-12-01

    A spectroscopic study of the dissolution of C60 and its monosubstituted derivatives methanofullerenes in 98% sulfuric acid revealed that methanofullerenes dissolved in sulfuric acid much better than the starting C60. A solubility series of functionalized fullerenes was obtained, which did not change during the extraction of methanofullerenes with sulfuric acid from benzene solutions. An effective methods was developed for separating methanofullerenes, which is based on the difference between the solubilities of the starting and functionalized fullerenes in concentrated sulfuric acid.

  18. The coagulation characteristics of humic acid by using acid-soluble chitosan, water-soluble chitosan, and chitosan coagulant mixtures.

    PubMed

    Chen, Chih-Yu; Wu, Chung-Yu; Chung, Ying-Chien

    2015-01-01

    Chitosan is a potential substitute for traditional aluminium salts in water treatment systems. This study compared the characteristics of humic acid (HA) removal by using acid-soluble chitosan, water-soluble chitosan, and coagulant mixtures of chitosan with aluminium sulphate (alum) or polyaluminium chloride (PACl). In addition, we evaluated their respective coagulation efficiencies at various coagulant concentrations, pH values, turbidities, and hardness levels. Furthermore, we determined the size and settling velocity of flocs formed by these coagulants to identify the major factors affecting HA coagulation. The coagulation efficiency of acid- and water-soluble chitosan for 15 mg/l of HA was 74.4% and 87.5%, respectively. The optimal coagulation range of water-soluble chitosan (9-20 mg/l) was broader than that of acid-soluble chitosan (4-8 mg/l). Notably, acid-soluble chitosan/PACl and water-soluble chitosan/alum coagulant mixtures exhibited a higher coagulation efficiency for HA than for PACl or alum alone. Furthermore, these coagulant mixtures yielded an acceptable floc settling velocity and savings in both installation and operational expenses. Based on these results, we confidently assert that coagulant mixtures with a 1:1 mass ratio of acid-soluble chitosan/PACl and water-soluble chitosan/alum provide a substantially more cost-effective alternative to using chitosan alone for removing HA from water. PMID:25362971

  19. Nitric acid uptake by sulfuric acid solutions under stratospheric conditions - Determination of Henry's Law solubility

    NASA Technical Reports Server (NTRS)

    Reihs, Christa M.; Golden, David M.; Tolbert, Margaret A.

    1990-01-01

    The uptake of nitric acid by sulfuric acid solutions representative of stratospheric particulate at low temperatures was measured to determine the solubility of nitric acid in sulfuric acid solutions as a function of H2SO4 concentration and solution temperature. Solubilities are reported for sulfuric acid solutions ranging from 58 to 87 wt pct H2SO4 over a temperature range from 188 to 240 K, showing that, in general, the solubility of nitric acid increases with decreasing sulfuric acid concentration and with decreasing temperature. The measured solubilities indicate that nitric acid in the global stratosphere will be found predominantly in the gas phase.

  20. Solid state stability and solubility of triethylenetetramine dihydrochloride.

    PubMed

    Henriet, Théo; Gana, Inès; Ghaddar, Carine; Barrio, Maria; Cartigny, Yohann; Yagoubi, Najet; Do, Bernard; Tamarit, Josep-Lluis; Rietveld, Ivo B

    2016-09-10

    The API triethylenetetramine dihydrochloride used as an alternative treatment of Wilson's disease is sensitive to water and it exhibits polymorphism. As this may become an issue for the drug formulation, the physical stability has been studied by differential scanning calorimetry, high-pressure thermal analysis, dynamic vapor sorption, and X-ray diffraction as a function of temperature. In addition, high-pressure liquid chromatography and mass spectrometry have been used to study the purity and chemical stability of the API. A pressure-temperature phase diagram of the pure compound has been constructed and it can be concluded that form II is monotropic in relation to form I, which is the only stable solid. The solubilities of the different solid forms have been determined with the help of a temperature - composition phase diagram. The API is very soluble, at 20° C about 10% of the saturated solution with respect to the dihydrate consists of API and the solubility of the pure form I is twice as high. Moreover, it has been shown that at 20°C, a relative humidity above 40% induces the formation of the dihydrate and at 70% a saturated solution appears. At higher temperatures, the formation of the dihydrate appears at lower relative humidity values. A clear link has been established between the API's chemical stability, its physical stability and the relative humidity in the air. Humidity levels above 40% are detrimental to the quality of the API. PMID:27377012

  1. Biorelevant solubility of poorly soluble drugs: rivaroxaban, furosemide, papaverine and niflumic acid.

    PubMed

    Takács-Novák, Krisztina; Szőke, Vera; Völgyi, Gergely; Horváth, Péter; Ambrus, Rita; Szabó-Révész, Piroska

    2013-09-01

    In this work the biorelevant solubility of four drugs representing different acid-base property, wide range of lipohilicity and low aqueous solubility was studied. The equilibrium solubility of rivaroxaban (non-ionizable), furosemide (acid), papaverine (base) and niflumic acid (ampholyte) was determined in simulated gastric fluid (SGF pH 1.2), in simulated intestinal fluid fasted state (FaSSIF pH 6.5) and fed state (FeSSIF pH 5.0) and their corresponding blank buffers at a temperature of 37 °C using saturation shake-flask method. The concentration was measured by optimized HPLC analysis. The solubilizing effect of bile acid/lipid micelles as additive components of biorelevent media (BRM) is expressed with the solubility ratio (SR: SBRM/Sblank buffer) and the food effect was estimated from SFeSSIF/SFaSSIF coefficient. It was revealed that ionization plays primarily role in solubility of compounds which undergo ionization in BRM. The solubilizing effect in FaSSIF was marginal for the neutral compound (rivaroxaban) and for molecules are anionic at pH 6.5 (furosemide and niflumic acid). The higher concentration of solubilizing agents in FeSSIF improved the solubility of papaverine carrying positive charge and niflumic acid being partially zwitterionic at pH 5.0. PMID:23770783

  2. Effect of ultrasound on the solubility limit of a sparingly soluble solid.

    PubMed

    Sandilya, D Krishna; Kannan, A

    2010-02-01

    The influence of power ultrasound (20kHz) on the rate of attainment of saturation of sparingly soluble benzoic acid in distilled water and in 24% (w/w) aqueous glycerol was experimentally investigated at 30 degrees C. The importance of proper temperature control of process vessel contents when it was irradiated with high ultrasonic power level settings was demonstrated. A method was proposed to calculate the volumetric mass transfer coefficient under non-isothermal conditions. PMID:19896884

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

    PubMed

    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. PMID:24329130

  4. Water and acid soluble trace metals in atmospheric particles

    NASA Technical Reports Server (NTRS)

    Lindberg, S. E.; Harriss, R. C.

    1983-01-01

    Continental aerosols are collected above a deciduous forest in eastern Tennessee and subjected to selective extractions to determine the water-soluble and acid-leachable concentrations of Cd, Mn, Pb, and Zn. The combined contributions of these metals to the total aerosol mass is 0.5 percent, with approximately 70 percent of this attributable to Pb alone. A substantial fraction (approximately 50 percent or more) of the acid-leachable metals is soluble in distilled water. In general, this water-soluble fraction increases with decreasing particle size and with increasing frequency of atmospheric water vapor saturation during the sampling period. The pattern of relative solubilities (Zn being greater than Mn, which is approximately equal to Cd, which is greater than Pb) is found to be similar to the general order of the thermodynamic solubilities of the most probable salts of these elements in continental aerosols with mixed fossil fuel and soil sources.

  5. Improvement in Aqueous Solubility of Retinoic Acid Receptor (RAR) Agonists by Bending the Molecular Structure.

    PubMed

    Hiramatsu, Michiaki; Ichikawa, Yuki; Tomoshige, Shusuke; Makishima, Makoto; Muranaka, Atsuya; Uchiyama, Masanobu; Yamaguchi, Takao; Hashimoto, Yuichi; Ishikawa, Minoru

    2016-08-01

    Aqueous solubility is a key requirement for many functional molecules, e. g., drug candidates. Decrease of the partition coefficient (log P) by chemical modification, i.e., introduction of hydrophilic group(s) into molecules, is a classical strategy for improving aqueous solubility. We have been investigating alternative strategies for improving the aqueous solubility of pharmaceutical compounds by disrupting intermolecular interactions. Here, we show that introducing a bend into the molecular structure of retinoic acid receptor (RAR) agonists by changing the substitution pattern from para to meta or ortho dramatically enhances aqueous solubility by up to 890-fold. We found that meta analogs exhibit similar hydrophobicity to the parent para compound, and have lower melting points, supporting the idea that the increase of aqueous solubility was due to decreased intermolecular interactions in the solid state as a result of the structural changes. PMID:27378357

  6. Solid solubility and diffusivity in an alumina/zirconia system

    SciTech Connect

    Stough, M.A.; Hellmann, J.R.

    1995-10-01

    Polycrystalline zirconia-coated single crystal sapphire fiber displays reconstruction of the sapphire surface in regions of contact with zirconia grains. This is a concern where ZrO{sub 2}-coated sapphire fiber is desired for reinforcement of ceramic matrices. Previous work has demonstrated pitting is partially attributed to impurity-induced transient liquid phase formation with local dissolution of alumina; however, the extent of reconstruction witnessed via microscopy suggests that other mechanisms are active. The present study has addressed the issue of solid solubility and interdiffusivity to more thoroughly understand the solid state mechanisms contributing to pitting. Single crystal sapphire and zirconia were ion implanted with zirconium and yttrium, and aluminum, respectively, and then subjected to diffusion anneals at 1,200--1,600 C to study redistribution of implanted cations. Secondary Ion Mass Spectroscopy (SIMS) was used to profile the redistribution of implanted ions for measurement of diffusion coefficients and solubility limits after heat treatments. The results will offer a significant set of data on interface stability in the alumina/zirconia system.

  7. Low acid producing solid propellants

    NASA Technical Reports Server (NTRS)

    Bennett, Robert R.

    1995-01-01

    The potential environmental effects of the exhaust products of conventional rocket propellants have been assessed by various groups. Areas of concern have included stratospheric ozone, acid rain, toxicity, air quality and global warming. Some of the studies which have been performed on this subject have concluded that while the impacts of rocket use are extremely small, there are propellant development options which have the potential to reduce those impacts even further. This paper discusses the various solid propellant options which have been proposed as being more environmentally benign than current systems by reducing HCI emissions. These options include acid neutralized, acid scavenged, and nonchlorine propellants. An assessment of the acid reducing potential and the viability of each of these options is made, based on current information. Such an assessment is needed in order to judge whether the potential improvements justify the expenditures of developing the new propellant systems.

  8. LITERATURE REVIEW OF BORIC ACID SOLUBILITY DATA

    SciTech Connect

    Crapse, K.; Kyser, E.

    2011-09-22

    A new solvent system is being evaluated for use in the Modular Caustic-Side Solvent Extraction Unit (MCU) and in the Salt Waste Processing Facility (SWPF). The new system replaces the current dilute nitric acid strip solution with 0.01 M boric acid. This literature study is performed to determine if there is a potential for boric acid to crystallize in the lines with emphasis on the transfer lines to the Defense Waste Processing Facility. This report focuses on the aqueous phase chemistry of boric acid under conditions relevant to MCU and SWPF. Operating and transfer conditions examined for the purpose of this review include temperatures between 13 C (McLeskey, 2008) and 45 C (Fondeur, 2007) and concentrations from 0 to 3M in nitric acid as well as exposure of small amounts of entrained boric acid in the organic phase to the sodium hydroxide caustic wash stream. Experiments were also conducted to observe any chemical reactions and off-gas generation that could occur when 0.01 M boric acid solution mixes with 3 M nitric acid solution and vice versa. Based on the low concentration (0.01M) of boric acid in the MCU/SWPF strip acid and the moderate operating temperatures (13 C to 45 C), it is unlikely that crystallization of boric acid will occur in the acid strip solution under process or transfer conditions. Mixing experiments of boric and nitric acid show no measurable gas generation (< 1 cc of gas per liter of solution) under similar process conditions.

  9. Solubility of HCL in sulfuric acid at stratospheric temperatures

    NASA Technical Reports Server (NTRS)

    Williams, Leah R.; Golden, David M.

    1993-01-01

    The solubility of HCl in sulfuric acid was measured using a Knudsen cell technique. Effective Henry's law constants are reported for sulfuric acid concentrations between 50 and 60 weight percent and for temperatures between 220 and 230 K. The measured values indicate that very little HCl will be dissolved in the stratospheric sulfate aerosol particles.

  10. Total soluble solids from banana: evaluation and optimization of extraction parameters.

    PubMed

    Carvalho, Giovani B M; Silva, Daniel P; Santos, Júlio C; Izário Filho, Hélcio J; Vicente, António A; Teixeira, José A; Felipe, Maria das Graças A; Almeida e Silva, João B

    2009-05-01

    Banana, an important component in the diet of the global population, is one of the most consumed fruits in the world. This fruit is also very favorable to industry processes (e.g., fermented beverages) due to its rich content on soluble solids and minerals, with low acidity. The main objective of this work was to evaluate the influence of factors such as banana weight and extraction time during a hot aqueous extraction process on the total soluble solids content of banana. The extract is to be used by the food and beverage industries. The experiments were performed with 105 mL of water, considering the moisture of the ripe banana (65%). Total sugar concentrations were obtained in a beer analyzer and the result expressed in degrees Plato (degrees P, which is the weight of the extract or the sugar equivalent in 100 g solution at 20 degrees C), aiming at facilitating the use of these results by the beverage industries. After previous studies of characterization of the fruit and of ripening performance, a 2(2) full-factorial star design was carried out, and a model was developed to describe the behavior of the dependent variable (total soluble solids) as a function of the factors (banana weight and extraction time), indicating as optimum conditions for extraction 38.5 g of banana at 39.7 min. PMID:19082923

  11. Solubility of acid gases in a mixed solvent

    SciTech Connect

    MacGregor, R.J.; Mather, A.E.

    1987-01-01

    The solubility of hydrogen sulphide and carbon dioxide and their mixtures has been measured at 40/sup 0/ and 100/sup 0/C in a mixed solvent consisting of 20.9 wt% (2.0 M) MDEA (methyldiethanolamine), 30.5 wt% sulfolane, and 48.6 wt% water. The results have been compared with those for aqueous 2.0 M MDEA and an analogous mixed solvent, containing AMP (2-amino-2-methyl-1-propanol), which are available in the literature. At solution loadings less than 1 mol acid gas/mol MDEA, the solubility of the acid gas was lower in the mixed solvent that in the corresponding aqueous MDEA solvent; at solution loadings greater than 1 mol acid gas/mol MDEA, the reverse was true. At all loadings and at both temperatures studied, the mixed MDEA solvent absorbed equal or lesser quantities of acid gas than the comparable mixed AMP solvent. However, the shapes of the solubility curves show that the mixed MDEA solvent would be a better choice for certain industrial applications. These data were used to modify the solubility model of Deshmukh and Mather to account for the mixed solvent effects on the system thermodynamics. Results show that the model is useful as a first approximation in predicting acid gas solubilities; agreement with experiment was generally found to be within +-15%.

  12. The removal of kaolinite suspensions by acid-soluble and water-soluble chitosans.

    PubMed

    Chung, Ying-Chien; Wu, Li-Chun; Chen, Chih-Yu

    2013-01-01

    Chitosan is a potential substitute for traditional aluminium salts in water treatment systems. This research compared the coagulant performance of acid-soluble chitosan with water-soluble chitosan and with coagulant mixtures of chitosan and aluminium sulfate (alum). We also assessed the coagulant performance of chitosan and poly-aluminium chloride (PAC) to remove kaolinite from turbid water. In addition, we evaluated their respective coagulation efficiencies under different coagulant concentrations, degrees of turbidity (NTU) and pH levels. Furthermore, we determined the size and settling velocity of flocs formed by these coagulants in order to illustrate major factors affecting kaolinite coagulation. The optimal concentrations of acid- versus water- soluble chitosan required to remove kaolinite from a 300 NTU suspension were 4.0 and 10.0 mg/l, respectively-with individual efficiencies of 79.3 and 92.4%, in that order. Optimum concentrations ofwater-soluble chitosan demonstrated a broader range than that of acid-soluble chitosan. In addition, it is of note that chitosan/alum and chitosan/PAC water-soluble coagulant mixtures demonstrated much wider ranges of optimal concentrations for turbidity reduction than either alum or PAC alone. Moreover, our water-soluble chitosan coagulant mixtures produced denser floc with elevated settling velocities that favour cost savings relevant to both installation and operational expenses. Based on our observations of these noteworthy performances, we confidently propose that a coagulant mixture with a 1:1 mass ratio of chitosan and alum presents a remarkably more cost-effective alternative to the use of chitosan alone in water treatment systems. PMID:23530342

  13. Leaching behavior and solubility -- Controlling solid phases of heavy metals in municipal solid waste incinerator ash

    SciTech Connect

    Johnson, C.A.; Ziegler, F.; Kersten, M.; Moor, H.C.

    1996-12-31

    This paper highlights the uses and limitations of thermodynamic calculations in the planning of leach tests in the laboratory or for research in the field. Heavy metal solubility has been studied in leachate from Landfill Lostorf, AG, Switzerland. Also, the influence of pH on the solubility of Cu, Pb, Cd and Zn has been determined in the laboratory. The results have been compared with the maximum allowable heavy metal concentrations in equilibrium with the appropriate (hydr)oxides and carbonates. Copper is supersaturated with respect to Cu(OH){sub 2} in both laboratory and field studies. Complexation with organic ligands is a probable explanation for this observation. Both Zn and Pb are undersaturated with respect to pure (hydr)oxides and carbonates, though agreement between calculations and measurements are close enough, that PbCO{sub 3} could be controlling the solubility in the laboratory experiments. The markedly lower concentrations of Pb in the field in comparison with the laboratory data could be explained by the affinity for Pb to bind to solids and the higher solid:solution ratio in field conditions. The solubility of Cd could be controlled by the formation of CdCO{sub 3}. The relatively high concentrations of Mo in the landfill leachate could be limited by the precipitation of CaMoO{sub 4}.

  14. Methane production and recovery using potato waste solubles and solids

    SciTech Connect

    Jackson, M.L.

    1982-01-01

    The production and recovery of methane gas utilizing various potato conversion wastes in either soluble or solid form is discussed in this chapter. Such wastes may occur at temperatures ranging from 25 C to as high as 55 C. The form and concentration of the waste and the temperature may dictate the choice of one of several possible treatment processes which are variously designated as conventional (holding tanks), contact (recycle of cell solids), and filter (packed bed) reactors. To this may be added a recent concept of an expanded bed reactor. A first design approach was employed to approximate capital and operating costs with an evaluation of the internal rates of return on investment and payout times. The fraction of the energy required by a processing plant which could be provided by the gas produced was of interest as a potential supplemental source of energy in the event that natural gas supplies are reduced or that prices of this fuel continue to escalate rapidly.

  15. Formation of water-soluble metal cyanide complexes from solid minerals by Pseudomonas plecoglossicida.

    PubMed

    Faramarzi, Mohammad A; Brandl, Helmut

    2006-06-01

    A few Pseudomonas species are able to form hydrocyanic acid (HCN), particularly when grown under glycine-rich conditions. In the presence of metals, cyanide can form water-soluble metal complexes of high chemical stability. We studied the possibility to mobilize metals as cyanide complexes from solid minerals using HCN-forming microorganisms. Pseudomonas plecoglossicida was cultivated in the presence of copper- and nickel-containing solid minerals. On powdered elemental nickel, fast HCN generation within the first 12 h of incubation was observed and water-soluble tetracyanaonickelate was formed. Cuprite, tenorite, chrysocolla, malachite, bornite, turquoise, millerite, pentlandite as well as shredded electronic scrap was also subjected to a biological treatment. Maximum concentrations of cyanide-complexed copper corresponded to a solubilization of 42% and 27% when P. plecoglossicida was grown in the presence of cuprite or tenorite, respectively. Crystal system, metal oxidation state and mineral hydrophobicity might have a significant influence on metal mobilization. However, it was not possible to allocate metal mobilization to a single mineral property. Cyanide-complexed gold was detected during growth on manually cut circuit boards. Maximum dicyanoaurate concentration corresponded to a 68.5% dissolution of the total gold added. These findings represent a novel type of microbial mobilization of nickel and copper from solid minerals based on the ability of certain microbes to form HCN. PMID:16684101

  16. Solubility calculations for acid gases in amine blends

    SciTech Connect

    Chakravarty, T.

    1985-01-01

    Treating with alkanolamines is often used to sweeten gases containing only a few parts per million of CO/sub 2/ and H/sub 2/S. Primary amines such as monoethanolamine (MEA) have great affinity for acid gases and are able to produce high purity sweet gas; on the other hand, tertiary amines like methyldiethanolamine (MDEA) have large capacity and are easy to regenerate but, because they do not bind chemically with CO/sub 2/, they are unable to produce a sweetened gas low in this component. Recently, the use of amine blends has become a subject of potentially great commercial importance. Since, the range of possible amines and blend formulations is large, a method for predicting equilibrium solubility is needed. A rigorous thermodynamic model has been developed which uses the extended Debye-Huckel expression, is very similar to one developed for single-amine solutions, and involves the fitting of binary interaction parameters to experimental data. In this work the interaction parameters found to be important in the activity coefficient expression were fitted to each single-acid-gas single-amine subsystem using all published solubility data. The resulting model was then validated by comparing mixed-acid-gas single-amine solubility predictions with published VLE data. MEA-MDEA and DEA-MDEA blends have been studied in detail in this work. It is found that each amine contributes to the overall acid gas solubility in a nonlinear way and that the solubility curves can exhibit maxima and minima as a function of the relative concentrations of the amines.

  17. The relationship between dissolved humic acids and soluble iron in estuaries

    NASA Technical Reports Server (NTRS)

    Fox, L. E.

    1984-01-01

    Dissolved humic acid and soluble iron appear to be chemically unassociated in estuaries despite their coincident removal. This conclusion is supported by differences in the aggregation kinetics of soluble iron and dissolved humic acid, the inability of extracted humic acid to stabilize laboratory preparations of ferric hydroxide, and decreasing ratios of humic acid carbon to soluble iron along the axes of some estuaries.

  18. A Soluble, Folded Protein without Charged Amino Acid Residues.

    PubMed

    Højgaard, Casper; Kofoed, Christian; Espersen, Roall; Johansson, Kristoffer Enøe; Villa, Mara; Willemoës, Martin; Lindorff-Larsen, Kresten; Teilum, Kaare; Winther, Jakob R

    2016-07-19

    Charges are considered an integral part of protein structure and function, enhancing solubility and providing specificity in molecular interactions. We wished to investigate whether charged amino acids are indeed required for protein biogenesis and whether a protein completely free of titratable side chains can maintain solubility, stability, and function. As a model, we used a cellulose-binding domain from Cellulomonas fimi, which, among proteins of more than 100 amino acids, presently is the least charged in the Protein Data Bank, with a total of only four titratable residues. We find that the protein shows a surprising resilience toward extremes of pH, demonstrating stability and function (cellulose binding) in the pH range from 2 to 11. To ask whether the four charged residues present were required for these properties of this protein, we altered them to nontitratable ones. Remarkably, this chargeless protein is produced reasonably well in Escherichia coli, retains its stable three-dimensional structure, and is still capable of strong cellulose binding. To further deprive this protein of charges, we removed the N-terminal charge by acetylation and studied the protein at pH 2, where the C-terminus is effectively protonated. Under these conditions, the protein retains its function and proved to be both soluble and have a reversible folding-unfolding transition. To the best of our knowledge, this is the first time a soluble, functional protein with no titratable side chains has been produced. PMID:27307139

  19. C-104 high-level waste solids: Washing/leaching and solubility versus temperature studies

    SciTech Connect

    GJ Lumetta; DJ Bates; JP Bramson; LP Darnell; OT Farmer III; SK Fiskum; LR Greenwood; FV Hoopes; CZ Soderquist; MJ Steele; RT Steele; MW Urie; JJ Wagner

    2000-05-17

    This report describes the results of a test conducted by Battelle to assess the effects of inhibited water washing and caustic leaching on the composition of the C-104 HLW solids. The objective of this work was to determine the composition of the C-104 solids remaining after washing with 0.01 M NaOH or leaching with 3 M NaOH. Another objective of this test was to determine the solubility of the C-104 solids as a function of temperature. The work was conducted according to test plan BNFL-TP-29953-8, Rev. 0, ``Determination of the Solubility of HLW Sludge Solids.

  20. Solubility Database

    National Institute of Standards and Technology Data Gateway

    SRD 106 IUPAC-NIST Solubility Database (Web, free access)   These solubilities are compiled from 18 volumes (Click here for List) of the International Union for Pure and Applied Chemistry(IUPAC)-NIST Solubility Data Series. The database includes liquid-liquid, solid-liquid, and gas-liquid systems. Typical solvents and solutes include water, seawater, heavy water, inorganic compounds, and a variety of organic compounds such as hydrocarbons, halogenated hydrocarbons, alcohols, acids, esters and nitrogen compounds. There are over 67,500 solubility measurements and over 1800 references.

  1. Solubility and dissolution enhancement of etoricoxib by solid dispersion technique using sugar carriers.

    PubMed

    Das, Abhisekh; Nayak, Amit Kumar; Mohanty, Biswaranjan; Panda, Satyabrata

    2011-01-01

    The aim of the present study was to improve solubility and dissolution of the poorly aqueous soluble drug, etoricoxib by solvent evaporation technique using various sugar carriers, such as lactose, sucrose, and mannitol. Etoricoxib solid dispersions and their respective physical mixtures using lactose, sucrose, and mannitol were prepared in different ratios by solvent evaporation technique. The percent yield, drug content, saturation solubility, and in vitro dissolution of etoricoxib solid dispersions and physical mixtures were analyzed. Etoricoxib solid dispersions were characterized by FTIR spectroscopy, XRD, and DSC analysis. The FTIR spectroscopic analysis revealed the possibility of intermolecular hydrogen bonding in various solid dispersions. The XRD and DSC studies indicated the transformation of crystalline etoricoxib (in pure drug) to amorphous etoricoxib (in solid dispersions) by the solid dispersion technology. Both the aqueous solubility and dissolution of etoricoxib were observed in all etoricoxib solid dispersions as compared with pure etoricoxib and their physical mixtures. The in vitro dissolution studies exhibited improved dissolution in case of solid dispersion using lactose than the solid dispersions using both sucrose and mannitol. The in vitro dissolution of etoricoxib from these solid dispersions followed Hixson-Crowell model. PMID:22389861

  2. Microemulsion formulation of clonixic acid: solubility enhancement and pain reduction.

    PubMed

    Lee, Jung-Mi; Park, Kyung-Mi; Lim, Soo-Jeong; Lee, Mi-Kyung; Kim, Chong-Kook

    2002-01-01

    Clonixic acid is currently marketed as a salt form because of its poor water-solubility. However, the commercial dosage form causes severe pain after intramuscular or intravenous injection. To improve the solubility of clonixic acid and to reduce pain on injection, clonixic acid was incorporated into oil-in-water microemulsions prepared from pre-microemulsion concentrate composed of varying ratios of oil and surfactant mixture. As an oil phase for drug incorporation, up to 14% castor oil could be included in the pre-microemulsion concentrate without a significant increase in droplet size. Both drug contents and droplet size increased as the weight ratio of Tween 20 to Tween 85 decreased. Taken together, when microemulsions were prepared from pre-microemulsion concentrate composed of 5:12:18 weight ratio of castor oil:Tween 20:Tween 85, clonixic acid could be incorporated at 3.2 mg mL(-1) in the microemulsion with a droplet size of less than 120 nm. The osmotic pressure of this microemulsion was remarkably lower than the commercial formulation, irrespective of the dilution ratios. The rat paw-lick test was used to compare pain responses among formulations. The microemulsion formulation significantly reduced the number of rats licking their paws as well as the total licking time, suggesting less pain induction by the microemulsion formulation. The pharmacokinetic parameters of clonixic acid after intravenous administration of the clonixic acid microemulsion to rats were not significantly different from those of the commercial formulation, lysine clonixinate. The present study suggests that microemulsion is an alternative formulation for clonixic acid with improved characteristics. PMID:11829128

  3. Proton conducting membrane using a solid acid

    NASA Technical Reports Server (NTRS)

    Chisholm, Calum (Inventor); Narayanan, Sekharipuram R. (Inventor); Boysen, Dane (Inventor); Haile, Sossina M. (Inventor)

    2002-01-01

    A solid acid material is used as a proton conducting membrane in an electrochemical device. The solid acid material can be one of a plurality of different kinds of materials. A binder can be added, and that binder can be either a nonconducting or a conducting binder. Nonconducting binders can be, for example, a polymer or a glass. A conducting binder enables the device to be both proton conducting and electron conducting. The solid acid material has the general form M.sub.a H.sub.b (XO.sub.t).sub.c.

  4. Improving the dissolution rate of poorly water soluble drug by solid dispersion and solid solution: pros and cons.

    PubMed

    Chokshi, Rina J; Zia, Hossein; Sandhu, Harpreet K; Shah, Navnit H; Malick, Waseem A

    2007-01-01

    The solid dispersions with poloxamer 188 (P188) and solid solutions with polyvinylpyrrolidone K30 (PVPK30) were evaluated and compared in an effort to improve aqueous solubility and bioavailability of a model hydrophobic drug. All preparations were characterized by differential scanning calorimetry, powder X-ray diffraction, intrinsic dissolution rates, and contact angle measurements. Accelerated stability studies also were conducted to determine the effects of aging on the stability of various formulations. The selected solid dispersion and solid solution formulations were further evaluated in beagle dogs for in vivo testing. Solid dispersions were characterized to show that the drug retains its crystallinity and forms a two-phase system. Solid solutions were characterized to be an amorphous monophasic system with transition of crystalline drug to amorphous state. The evaluation of the intrinsic dissolution rates of various preparations indicated that the solid solutions have higher initial dissolution rates compared with solid dispersions. However, after storage at accelerated conditions, the dissolution rates of solid solutions were lower due to partial reversion to crystalline form. The drug in solid dispersion showed better bioavailability in comparison to solid solution. Therefore, considering physical stability and in vivo study results, the solid dispersion was the most suitable choice to improve dissolution rates and hence the bioavailability of the poorly water soluble drug. PMID:17107929

  5. Phase Behavior of Complex Superprotonic Solid Acids

    NASA Astrophysics Data System (ADS)

    Panithipongwut, Chatr

    Superprotonic phase transitions and thermal behaviors of three complex solid acid systems are presented, namely Rb3H(SO4) 2-RbHSO4 system, Rb3H(SeO4)2-Cs 3H(SeO4)2 solid solution system, and Cs6 (H2SO4)3(H1.5PO4) 4. These material systems present a rich set of phase transition characteristics that set them apart from other, simpler solid acids. A.C. impedance spectroscopy, high-temperature X-ray powder diffraction, and thermal analysis, as well as other characterization techniques, were employed to investigate the phase behavior of these systems. Rb3H(SO4)2 is an atypical member of the M3H(XO4)2 class of compounds (M = alkali metal or NH4+ and X = S or Se) in that a transition to a high-conductivity state involves disproportionation into two phases rather than a simple polymorphic transition [1]. In the present work, investigations of the Rb3H(SO4)2-RbHSO4 system have revealed the disproportionation products to be Rb2SO 4 and the previously unknown compound Rb5H3(SO 4)4. The new compound becomes stable at a temperature between 25 and 140 °C and is isostructural to a recently reported trigonal phase with space group P3m of Cs5H 3(SO4)4 [2]. At 185 °C the compound undergoes an apparently polymorphic transformation with a heat of transition of 23.8 kJ/mol and a slight additional increase in conductivity. The compounds Rb3H(SeO4)2 and Cs 3H(SeO4)2, though not isomorphous at ambient temperatures, are quintessential examples of superprotonic materials. Both adopt monoclinic structures at ambient temperatures and ultimately transform to a trigonal (R3m) superprotonic structure at slightly elevated temperatures, 178 and 183 °C, respectively. The compounds are completely miscible above the superprotonic transition and show extensive solubility below it. Beyond a careful determination of the phase boundaries, we find a remarkable 40-fold increase in the superprotonic conductivity in intermediate compositions rich in Rb as compared to either end-member. The compound Cs6(H2

  6. Solubility enhancement of lovastatin by modified locust bean gum using solid dispersion techniques.

    PubMed

    Patel, Manjil; Tekade, Avinash; Gattani, Surendra; Surana, Sanjay

    2008-01-01

    The aim of the present study was to improve the solubility of poorly water soluble drug lovastatin (LS) by solid dispersion (SD) techniques using modified locust bean gum (MLBG) as a carrier. The locust bean gum (LBG) was modified by heating and there observed irreversible decrease in viscosity, whereas swelling property remains unaffected. The advantage of modification of LBG was illustrated by difference in dissolution profiles of their SD. Effect of polymer concentration and methods of preparation on solubility enhancement were studied using solubility and dissolution studies, respectively. The result of solubility study showed increase in solubility of LS with increase in concentration of MLBG. It was found that the dissolution rate of LS from its SD was dependent on the method of preparation of solid dispersions. Dissolution study revealed that the modified solvent evaporation is most convenient and effective method for solubility enhancement of poorly water soluble drug LS, among various methods of preparation of SD. The prepared SDs were characterized by differential scanning calorimetry, scanning electron microscopy, and X-ray diffraction study. In vivo study was performed by measuring 3-hydroxy-3-methyl-glutaryl-coenzyme A (HMG Co-A) reductase inhibition activity. Significant reduction in HMG Co-A reductase activity was observed in case of solid dispersions of LS than plain LS. In conclusion, MLBG could be used as a potential carrier in enhancing the dissolution rate and bioavailability of LS. PMID:19115112

  7. Predicting the solid solubility limit in high-entropy alloys using the molecular orbital approach

    NASA Astrophysics Data System (ADS)

    Sheikh, Saad; Klement, Uta; Guo, Sheng

    2015-11-01

    High-entropy alloys (HEAs) are currently at the research frontier of metallic materials. Understanding the solid solubility limit in HEAs, such a highly concentrated multicomponent alloy system, is scientifically intriguing. It is also technically important to achieve desirable mechanical properties by controlling the formation of topologically or geometrically closed packed phases. Previous approaches to describe the solid solubilities in HEAs could not accurately locate the solubility limit and have to utilize at least two parameters. Here, we propose to use a single parameter, the average energy of d-orbital levels, Md, to predict the solid solubility limit in HEAs. It is found that Md can satisfactorily describe the solid solubilities in fcc structured HEAs containing 3 d transition metals, and also in bcc structured HEAs. This finding will greatly simplify the alloys design and lends more flexibility to control the mechanical properties of HEAs. When 4 d transition metals are alloyed, Md alone cannot describe the solid solubility limit in fcc structured HEAs, due to the large increase of the bond strength that can be gauged by the bond order, Bo. The potential opportunities and challenges with applying the molecular orbital approach to HEAs are discussed.

  8. Proton conducting membrane using a solid acid

    NASA Technical Reports Server (NTRS)

    Haile, Sossina M. (Inventor); Chisholm, Calum (Inventor); Boysen, Dane A. (Inventor); Narayanan, Sekharipuram R. (Inventor)

    2006-01-01

    A solid acid material is used as a proton conducting membrane in an electrochemical device. The solid acid material can be one of a plurality of different kinds of materials. A binder can be added, and that binder can be either a nonconducting or a conducting binder. Nonconducting binders can be, for example, a polymer or a glass. A conducting binder enables the device to be both proton conducting and electron conducting.

  9. IUPAC-NIST Solubility Data Series. 99. Solubility of Benzoic Acid and Substituted Benzoic Acids in Both Neat Organic Solvents and Organic Solvent Mixtures

    NASA Astrophysics Data System (ADS)

    Acree, William E.

    2013-09-01

    Solubility data are compiled and reviewed for benzoic acid and 63 substituted benzoic acids dissolved in neat organic solvents and well-defined binary and ternary organic solvent mixtures. The compiled solubility data were retrieved from the published chemical and pharmaceutical literature covering the period from 1900 to the beginning of 2013.

  10. Superprotonic solid acids: Structure, properties, and applications

    NASA Astrophysics Data System (ADS)

    Boysen, Dane Andrew

    In this work, the structure and properties of superprotonic MH nXO4-type solid acids (where M = monovalent cation, X = S, Se, P, As, and n = 1, 2) have been investigated and, for the first time, applied in fuel cell devices. Several MH nXO4-type solid acids are known to undergo a "superprotonic" solid-state phase transition upon heating, in which the proton conductivity increases by several orders of magnitude and takes on values of ˜10 -2O-1cm-1. The presence of superprotonic conductivity in fully hydrogen bonded solid acids, such as CsH2PO4, has long been disputed. In these investigations, through the use of pressure, the unequivocal identification of superprotonic behavior in both RbH2PO4 and CsH2PO 4 has been demonstrated, whereas for chemically analogous compounds with smaller cations, such as KH2PO4 and NaH2PO 4, superprotonic conductivity was notably absent. Such observations have led to the adoption of radius ratio rules, in an attempt to identify a critical ion size effect on the presence of superprotonic conductivity in solid acids. It has been found that, while ionic size does play a prominent role in the presence of superprotonic behavior in solid acids, equally important are the effects of ionic and hydrogen bonding. Next, the properties of superprotonic phase transition have been investigated from a thermodynamic standpoint. With contributions from this work, a formulation has been developed that accounts for the entropy resulting from both the disordering of both hydrogen bonds and oxy-anion librations in the superprotonic phase of solid acids. This formulation, fundamentally derived from Linus Pauling's entropy rules for ice, accurately accounts for the change in entropy through a superprotonic phase transition. Lastly, the first proof-of-priniciple fuel cells based upon solid acid electrolytes have been demonstrated. Initial results based upon a sulfate electrolyte, CsHSO4, demonstrated the viability of solid acids, but poor chemical stability

  11. Superprotonic Solid Acids Thermochemistry, Structure, and Conductivity

    NASA Astrophysics Data System (ADS)

    Ikeda, Ayako

    In this work, in order to investigate the thermochemistry and property of the superprotonic solid acid compounds, the measurement methods were established for in situ observation, because superprotonic phases are neither stable at room temperature nor freezable to room temperature. A humidity-controlled TG, DSC and AC impedance measurement system, and high temperature stage for XRD were built for thermal analysis and characterization of the solid acid compounds. The thermodynamic and kinetics of the dehydration and hydration of CsH 2PO4 is investigated by TG, DSC, and XRD analysis. By making use of the enhanced kinetics afforded by SiO2, the phase boundary between CsH2PO4, CsPO3, and dehydrated liquid was precisely determined. The stability of CsH2PO4 and the liquid dehydrate, CsH2(1-x)PO4-x(l), were confirmed by the complete reversal of dehydration to recover these phases in the appropriate temperature and water partial pressure ranges. Rehydration and conversion of CsPO3(s) to CsH2PO4(s) occurs over a period of several hours, depending on temperature, water partial pressure, and morphology of the metaphosphate. High and small particles favor rapid dehydration, whereas the temperature dependence of the rehydration kinetics is nonmonotonic, reaching its fastest rate in the vicinity of the superprotonic transition. Doping Rb and K into CDP was examined and the stable region of Cs 1-xRbxH2PO4 and Cs1-xKxH2PO 4 are determined by in situ XRD and DSC measurement. Then the effects of doping to the structure and conductivity are discussed. It was found that Rb has whole-range solubility for both cubic and monoclinic CDP. Ts increases and Td decrease with Rb content. K has 27% solubility for cubic CDP, T s and Td decrease with K content. The eutectic temperature is 208 +/- 2°C. The lattice size of Rb- or K- doped CDP depends on the averaged cation size. Conductivity linearly decreases by dopant concentration. The impact of K doping is deeper than that of Rb for the

  12. Physical stability of solid dispersions with respect to thermodynamic solubility of tadalafil in PVP-VA.

    PubMed

    Wlodarski, K; Sawicki, W; Kozyra, A; Tajber, L

    2015-10-01

    The aim of this paper was to evaluate physical stability of solid dispersions in respect to the drug, tadalafil (Td), in vinylpyrrolidone and vinyl acetate block copolymer (PVP-VA). Nine solid dispersions of Td in PVP-VA (Td/PVP-VA) varied in terms of quantitative composition (1:9-9:1, w/w) were successfully produced by spray-drying. Their amorphous nature, supersaturated character and molecular level of mixing (a solid solution structure) were subsequently confirmed using DSC, PXRD, SEM and calculation of Hansen total solubility parameters. Due to thermal degradation of both components before the melting point of Td (302.3°C), an approach based on the drug crystallization from the supersaturated solid dispersion was selected to calculate the solubility of Td in the polymer. Annealing of the Td/PVP-VA solid dispersion (1:1, w/w) at selected temperatures above its Tg resulted in different stable solid dispersions. According to the Gordon-Taylor equation their new Tgs gave the information about the quantitative composition which corresponded to the thermodynamic solubility of Td in PVP-VA at given temperatures of annealing. The obtained relationship was fitted to the exponential function, with the calculated solubility of Td of 20.5% at 25°C. This value was in accordance with the results of hot stage polarizing light microscopy as well as stability tests carried out at 80°C and 0% RH, in which Td solid dispersions containing 10-20% of the drug were the only systems that did not crystallize within two months. A thermal analysis protocol utilizing a fast heating rate was shown to generate Td solubility data complementing the solid dispersion method. The Flory-Huggins model applied for the Td/PVP-VA system yielded the solubility value of 0.1% at 25°C, showing the lack of applicability in this case. PMID:26247119

  13. Solid Solubilities of Pu, U, Gd and Hf in Candidate Ceramic Nuclear Wasteforms

    SciTech Connect

    Vance, Eric R.; Carter, M. L.; Lumpkin, G. R.; Day, R. A.; Begg, B. D.

    2001-04-02

    This goal of this research project was to determine the solid solubility of Pu, U, Gd, and Hf in candidate ceramics for immobilization of high-level nuclear waste. The experimental approach was to saturate each phase by adding more than the solid solubility limit of the given cation, using a nominated substitution scheme, and then analyzing the candidate phase that formed to evaluate the solid solubility limit under firing conditions. Confirmation that the solid solution limit had been reached insofar as other phases rich in the cation of interest was also required. The candidate phases were monazite, titanite, zirconolite, perovskite, apatite, pyrochlore, and brannerite. The valences of Pu and U were typically deduced from the firing atmosphere, and charge balancing in the candidate phase composition as evaluated from electron microscopy, although in some cases it was measured directly by x-ray absorption and diffuse reflectance spectroscopies (for U). Tetravalent Pu and U have restricted (< 0.1 formula units) solid solubility in apatite, titanite, and perovskite. Trivalent Pu has a larger solubility in apatite and perovskite than Pu4+. U3+ appears to be a credible species in reduced perovskite with a solubility of {approximately} 0.25 f.u. as opposed to {approximately} 0.05 f.u. for U4+. Pu4+ is a viable species in monazite and is promoted at lower firing temperatures ({approximately} 800 C) in an air atmosphere. Hf solubility is restricted in apatite, monazite (< 0.1 f.u.), but is {approximately} 0.2 and 0.5 f.u. in brannerite and titanite, respectively. Gd solubility is extended in all phases except for titanite ({approximately} 0.3 f.u.). U5+ was identified by DRS observations of absorption bands in the visible/near infrared photon energy ranges in brannerite and zirconolite, and U4+ in zirconolite was similarly identified.

  14. Benzoic acid 2-hydroxylase, a soluble oxygenase from tobacco, catalyzes salicylic acid biosynthesis

    SciTech Connect

    Leon, J.; Shulaev, V.; Yalpani, N.

    1995-10-24

    Benzoic acid 2-hydroxylase (BA2H) catalyzes the biosynthesis of salicylic acid from benzoic acid. The enzyme has been partially purified and characterized as a soluble protein of 160 kDa. High-efficiency in vivo labeling of salicyclic acid with {sup 18}O{sub 2} suggested that BA2H is an oxygenase that specifically hydroxylates the ortho position of benzoic acid. The enzyme was strongly induced by either tobacco mosaic virus inoculation of benzoic acid infiltration of tobacco leaves and it was inhibited by CO and other inhibitors of cytochrome P450 hydroxylases. The BA2H activity was immunodepleted by antibodies raised against SU2, a soluble cytochrome P450 from Streptomyces griseolus. The anti-SU2 antibodies immunoprecipitated a radiolabeled polypeptide of around 160 kDa from the soluble protein extracts of L-[{sup 35}S]-methionine-fed tobacco leaves. Purified BA2H showed CO-difference spectra with a maximum at 457 nm. These data suggest that BA2H belongs to a novel class of soluble, high molecular weight cytochrome P450 enzymes. 21 refs., 6 figs., 1 tab.

  15. Wet spinning of solid polyamic acid fibers

    NASA Technical Reports Server (NTRS)

    Dorogy, William E., Jr. (Inventor); St.clair, Anne K. (Inventor)

    1991-01-01

    The invention is a process for the production of solid aromatic polyamic acid and polyimide fibers from a wet gel or coagulation bath wet gel using N,N-dimethylacetamide (DMAc) solutions of the polyamic acid derived from aromatic dianhydrides such as 3,3',4,4' benzophenonetetra carboxylic dianhydride (BTDA) and aromatic diamines such as 4,4'-oxydianiline (4,4'-ODA). By utilizing the relationship among coagulation medium and concentration, resin inherent viscosity, resin percent solids, filament diameter, and fiber void content, it is possible to make improved polyamic acid fibers. Solid polyimide fibers, obtained by the thermal cyclization of the polyamic acid precursor, have increased tensile properties compared to fibers containing macropores from the same resin system.

  16. Water-enhanced solubility of carboxylic acids in organic solvents and its applications to extraction processes

    SciTech Connect

    Starr, J.N.; King, C.J.

    1991-11-01

    The solubilities of carboxylic acids in certain organic solvents increase remarkably with an increasing amount of water in the organic phase. This phenomenon leads to a novel extract regeneration process in which the co-extracted water is selectively removed from an extract, and the carboxylic acid precipitates. This approach is potentially advantageous compared to other regeneration processes because it removes a minor component of the extract in order to achieve a large recovery of acid from the extract. Carboxylic acids of interest include adipic acid, fumaric acid, and succinic acid because of their low to moderate solubilities in organic solvents. Solvents were screened for an increase in acid solubility with increased water concentration in the organic phase. Most Lewis-base solvents were found to exhibit this increased solubility phenomena. Solvents that have a carbonyl functional group showed a very large increase in acid solubility. 71 refs., 52 figs., 38 tabs.

  17. [Partial least squares regression variable screening studies on apple soluble solids NIR spectral detection].

    PubMed

    Ouyang, Ai-Guo; Xie, Xiao-Qiang; Zhou, Yan-Rui; Liu, Yan-De

    2012-10-01

    Abstract To improve the predictive ability and robustness of the NIR correction model of the soluble solid content (SSC) of apple, the reverse interval partial least squares method, genetic algorithm and the continuous projection method were implemented to select variables of the NIR spectroscopy of the soluble solid content (SSC) of apple, and the partial least squares regression model was established. By genetic algorithm for screening of the 141 variables of the correction model, prediction has the best effect. And compared to the full spectrum correction model, the correlation coefficient increased to 0.96 from 0.93, forecast root mean square error decreased from 0.30 degrees Brix to 0.23 degrees Brix. This experimental results show that the genetic algorithm combined with partial least squares regression method improved the detection precision of the NIR model of the soluble solid content (SSC) of apple. PMID:23285864

  18. Bioavailability enhancement of a poorly water-soluble drug by solid dispersion in polyethylene glycol-polysorbate 80 mixture.

    PubMed

    Joshi, Hemant N; Tejwani, Ravindra W; Davidovich, Martha; Sahasrabudhe, Vaishali P; Jemal, Mohammed; Bathala, Mohinder S; Varia, Sailesh A; Serajuddin, Abu T M

    2004-01-01

    Oral bioavailability of a poorly water-soluble drug was greatly enhanced by using its solid dispersion in a surface-active carrier. The weakly basic drug (pK(a) approximately 5.5) had the highest solubility of 0.1mg/ml at pH 1.5, < 1 microg/ml aqueous solubility between pH 3.5 and 5.5 at 24+/-1 degrees C, and no detectable solubility (< 0.02 microg/ml) at pH greater than 5.5. Two solid dispersion formulations of the drug, one in Gelucire 44/14 and another one in a mixture of polyethylene glycol 3350 (PEG 3350) with polysorbate 80, were prepared by dissolving the drug in the molten carrier (65 degrees C) and filling the melt in hard gelatin capsules. From the two solid dispersion formulations, the PEG 3350-polysorbate 80 was selected for further development. The oral bioavailability of this formulation in dogs was compared with that of a capsule containing micronized drug blended with lactose and microcrystalline cellulose and a liquid solution in a mixture of PEG 400, polysorbate 80 and water. For intravenous administration, a solution in a mixture of propylene glycol, polysorbate 80 and water was used. Absolute oral bioavailability values from the capsule containing micronized drug, the capsule containing solid dispersion and the oral liquid were 1.7+/-1.0%, 35.8+/-5.2% and 59.6+/-21.4%, respectively. Thus, the solid dispersion provided a 21-fold increase in bioavailability of the drug as compared to the capsule containing micronized drug. A capsule formulation containing 25 mg of drug with a total fill weight of 600 mg was subsequently selected for further development. The selected solid dispersion formulation was physically and chemically stable under accelerated storage conditions for at least 6 months. It is hypothesized that polysorbate 80 ensures complete release of drug in a metastable finely dispersed state having a large surface area, which facilitates further solubilization by bile acids in the GI tract and the absorption into the enterocytes. Thus, the

  19. Effects of CO2 enrichment on the metabolism of soluble amino acids and organic acids in barley primary leaves

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Responses of soluble amino acids and organic acids to CO2 enrichment were determined with barley primary leaves (Hordeum vulgare L. cv. Brant) grown in controlled environment chambers. Total soluble amino acids were enhanced 33% by CO2 enrichment when determined 9 days after sowing (DAS). However,...

  20. Uptake of Hypobromous Acid (HOBr) by Aqueous Sulfuric Acid Solutions: Low-Temperature Solubility and Reaction

    NASA Technical Reports Server (NTRS)

    Iraci, Laura T.; Michelsen, Rebecca R.; Ashbourn, Samatha F. M.; Rammer, Thomas A.; Golden, David M.

    2005-01-01

    Hypobromous acid (HOBr) is a key species linking inorganic bromine to the chlorine and odd hydrogen chemical families. We have measured the solubility of HOBr in 45 - 70 wt% sulfuric acid solutions representative of upper tropospheric and lower stratospheric aerosol composition. Over the temperature range 201 - 252 K, HOBr is quite soluble in sulfuric acid, with an effective Henry's law coefficient, H* = 10(exp 4) - 10(exp 7) mol/L/atm. H* is inversely dependent on temperature, with Delta H = -46.2 kJ/mol and Delta S = -106.2 J/mol/K for 55 - 70 wt% H2SO4 solutions. Our study includes temperatures which overlap both previous measurements of HOBr solubility. For uptake into aqueous 45 wt% H2SO4, the solubility can be described by log H* = 3665/T - 10.63. For 55 - 70 wt% H2SO4, log H* = 2412/T - 5.55. At temperatures colder than approx. 213 K, the solubility of HOBr in 45 wt% H2SO4 is noticeably larger than in 70 wt% H2SO4. The solubility of HOBr is comparable to that of HBr, indicating that upper tropospheric and lower stratospheric aerosols should contain equilibrium concentrations of HOBr which equal or exceed those of HBr. Our measurements indicate chemical reaction of HOBr upon uptake into aqueous sulfuric acid in the presence of other brominated gases followed by evolution of gaseous products including Br2O and Br2, particularly at 70 wt% H2SO4.

  1. Comparative study on solid self-nanoemulsifying drug delivery and solid dispersion system for enhanced solubility and bioavailability of ezetimibe

    PubMed Central

    Rashid, Rehmana; Kim, Dong Wuk; Yousaf, Abid Mehmood; Mustapha, Omer; Din, Fakhar ud; Park, Jong Hyuck; Yong, Chul Soon; Oh, Yu-Kyoung; Youn, Yu Seok; Kim, Jong Oh; Choi, Han-Gon

    2015-01-01

    Background The objective of this study was to compare the physicochemical characteristics, solubility, dissolution, and oral bioavailability of an ezetimibe-loaded solid self-nanoemulsifying drug delivery system (SNEDDS), surface modified solid dispersion (SMSD), and solvent evaporated solid dispersion (SESD) to identify the best drug delivery system with the highest oral bioavailability. Methods For the liquid SNEDDS formulation, Capryol 90, Cremophor EL, and Tween 80 were selected as the oil, surfactant, and cosurfactant, respectively. The nanoemulsion-forming region was sketched using a pseudoternary phase diagram on the basis of reduced emulsion size. The optimized liquid SNEDDS was converted to solid SNEDDS by spray drying with silicon dioxide. Furthermore, SMSDs were prepared using the spray drying technique with various amounts of hydroxypropylcellulose and Tween 80, optimized on the basis of their drug solubility. The SESD formulation was prepared with the same composition of optimized SMSD. The aqueous solubility, dissolution, physicochemical properties, and pharmacokinetics of all of the formulations were investigated and compared with the drug powder. Results The drug existed in the crystalline form in SMSD, but was changed into an amorphous form in SNEDDS and SESD, giving particle sizes of approximately 24, 6, and 11 µm, respectively. All of these formulations significantly improved the aqueous solubility and dissolution in the order of solid SNEDDS ≥ SESD > SMSD, and showed a total higher plasma concentration than did the drug powder. Moreover, SESD gave a higher area under the drug concentration time curve from zero to infinity than did SNEDDS and SMSD, even if they were not significantly different, suggesting more improved oral bioavailability. Conclusion Among the various formulations tested in this study, the SESD system would be strongly recommended as a drug delivery system for the oral administration of ezetimibe with poor water solubility

  2. IUPAC-NIST Solubility Data Series. 90. Hydroxybenzoic Acid Derivatives in Binary and Ternary Systems. Part II. Hydroxybenzoic Acids, Hydroxybenzoates, and Hydroxybenzoic Acid Salts in Nonaqueous Systems

    NASA Astrophysics Data System (ADS)

    Goto, Ayako; Miyamoto, Hiroshi; Salomon, Mark; Goto, Rensuke; Fukuda, Hiroshi; Königsberger, Erich; Königsberger, Lan-Chi; Scharlin, Pirketta

    2011-06-01

    The solid-liquid solubility data for well defined nonaqueous binary and ternary systems are reviewed. One component includes hydroxybenzoic acid, hydroxybenzoate, and hydroxybenzoic acid salt, and another component includes a variety of organic compounds (hydrocarbons, alcohols, halogenated hydrocarbons, carboxylic acids, esters, et al.) and carbon dioxide. The ternary systems include mixtures of organic substances of various classes and carbon dioxide. The total number of compilation sheets is 270 for six types of system. Almost all data are expressed as mass percent and mole fraction as well as the originally reported units, while some data are expressed as molar concentration. Critical evaluation was carried out for the binary nonaqueous systems of 2-, 3-, and 4-hydroxybenzoic acids and hydroxybenzoates (methylparaben, ethylparaben, propylparaben, and butylparaben) in alcohols, 1-heptane, and benzene.

  3. The effects of acid treatment and calcium ions on the solubility of concanavalin A

    NASA Technical Reports Server (NTRS)

    Cacioppo, Elizabeth; Pusey, Marc L.

    1992-01-01

    The effects of acid treatment (which removes Mn and Ca ions) and Ca(2+) ions on the solubility of jack-bean-meal concanavalin A were investigated using two techniques: the sitting drop technique and the microcolumn technique. It was found that the solubility of concanavalin A varied with the protein preparation procedures and with measurement techniques. Addition of Ca(2+) resulted in greatly lowered solubilities compared with the acid treated protein. The sitting drop solubilities for the recalcified protein agreed better with those reported by Mikol and Giege (1989) than with solubilities determined from column data.

  4. SOLUBLE SOLIDS AND SIMPLE SUGARS MEASUREMENT IN INTACT MANGO USING NEAR INFRARED SPECTROSCOPY

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Total soluble solids content (TSS, °Brix), sucrose, glucose and fructose are important quality attributes of mango (Magnifera indica) fruit and have been shown to be useful for determining fruit maturity. The approach to develop a rapid, reliable, nondestructive method for quality evaluation of man...

  5. Potassium application to table grape clusters after veraison increases soluble solids by enhancing berry water loss

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Potassium salt solutions were applied twice to clusters of several table grapes cultivars, after the onset of veraison and three weeks later. Potassium bicarbonate, potassium sorbate, and glycine-complexed potassium, a commercial fertilizer product, increased soluble solids content consistently, whi...

  6. Comparison and fusion of four nondestructive sensors for predicting apple fruit firmness and soluble solids content

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Four nondestructive technologies (i.e., acoustic firmness, bioyield firmness, visible/near-infrared (NIR) spectroscopy, and spectral scattering) have been developed in recent years for assessing the firmness and/or soluble solids content (SSC) of apples. Each of these technologies has its merits and...

  7. Analysis of Hyperspectral Scattering Characteristics for Predicting Apple Fruit Firmness and Soluble Solids Content

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Spectral scattering is useful for assessing the firmness and soluble solids content (SSC) of apples because it provides an effective means for characterizing light scattering in the fruit. This research compared three methods for quantifying the spectral scattering profiles acquired from ‘Golden Del...

  8. Effects of ground corn particle size on ethanol yield and thin stillage soluble solids

    Technology Transfer Automated Retrieval System (TEKTRAN)

    The effects of ground corn particle size on ethanol yield and soluble solids in thin stillage were evaluated using a 2-L laboratory dry-grind procedure. The procedure was optimized for grinding, liquefaction, saccharification, and fermentation parameters. The optimized procedure was reproducible wi...

  9. Multi-sensor Data Fusion for Improved Prediction of Apple Fruit Firmness and Soluble Solids Content

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Several nondestructive technologies have been developed for assessing the firmness and soluble solids content (SSC) of apples. Each of these technologies has its merits and limitations in predicting these quality parameters. With the concept of multi-sensor data fusion, different sensors would work ...

  10. Optimal Wavelengths Selection for Hyperspectral Scattering Prediction of Apple Firmness and Soluble Solids Content

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Hyperspectral scattering is a promising technique for nondestructive quality measurement of apple fruit, and extraction of the most useful information from the hyperspectral scattering data is critical to accurate assessment of fruit firmness and soluble solids content (SSC). A hierarchical evolutio...

  11. Development, characterization and solubility study of solid dispersions of Cefuroxime Axetil by the solvent evaporation method

    PubMed Central

    Arora, S. C.; Sharma, P. K.; Irchhaiya, Raghuveer; Khatkar, Anurag; Singh, Neeraj; Gagoria, Jagbir

    2010-01-01

    Cefuroxime Axetil (Poorly water soluble drug), when prepared as solid dispersion showed improved solubility and dissolution. Therefore, the main purpose of this investigation was to increase the solubility and dissolution rate of Cefuroxime Axetil by the preparation of its solid dispersion with urea, using the solvent evaporation method. Physical mixtures and solid dispersions of Cefuroxime Axetil were prepared by using urea as a water-soluble carrier in various proportions (1:1, 1:2, 1:3, 1:4, 1:5, 1:6, and 1:7 by weight), by employing the solvent evaporation method. The drug release profile was studied and it was found that the dissolution rate and the dissolution parameters of the drug from the physical mixture as well as solid dispersion were higher than those of the intact drug. The Fourier Transform Infrared (FTIR) spectra revealed no chemical incompatibility between the drug and urea. Drug-polymer interactions were investigated using differential scanning calorimetry (DSC) and Powder X-Ray Diffraction (PXRD). PMID:22247865

  12. DEVELOPMENT, CHARACTERIZATION AND SOLUBILITY STUDY OF SOLID DISPERSIONS OF AZITHROMYCIN DIHYDRATE BY SOLVENT EVAPORATION METHOD

    PubMed Central

    Arora, S.C.; Sharma, P.K.; Irchhaiya, Raghuveer; Khatkar, Anurag; Singh, Neeraj; Gagoria, Jagbir

    2010-01-01

    Azithromycin Dihydrate (Poorly water soluble drug), when prepared as solid dispersion showed improved solubility and dissolution. So the main purpose of this investigation was to increase the solubility and dissolution rate of Azithromycin Dihydrate by the preparation of its solid dispersion with urea using solvent evaporation method. Physical mixtures and solid dispersions of Azithromycin Dihydrate were prepared by using urea as water-soluble carrier in various proportions (1:1, 1:2, 1:3, 1:4, 1:5, 1:6, 1:7 by weight), by employing solvent evaporation method. The drug release profile was studied and it was found that the dissolution rate and the dissolution parameters of the drug from the physical mixture as well as solid dispersion were higher than those of the intact drug. FT- IR spectra revealed no chemical incompatibility between drug and urea. Drug-polymer interactions were investigated using differential scanning calorimetry (DSC) and Powder X-Ray Diffraction (PXRD). PMID:22247849

  13. Porous Silica-Supported Solid Lipid Particles for Enhanced Solubilization of Poorly Soluble Drugs.

    PubMed

    Yasmin, Rokhsana; Rao, Shasha; Bremmell, Kristen E; Prestidge, Clive A

    2016-07-01

    Low dissolution of drugs in the intestinal fluid can limit their effectiveness in oral therapies. Here, a novel porous silica-supported solid lipid system was developed to optimize the oral delivery of drugs with limited aqueous solubility. Using lovastatin (LOV) as the model poorly water-soluble drug, two porous silica-supported solid lipid systems (SSL-A and SSL-S) were fabricated from solid lipid (glyceryl monostearate, GMS) and nanoporous silica particles Aerosil 380 (silica-A) and Syloid 244FP (silica-S) via immersion/solvent evaporation. SSL particles demonstrated significantly higher rate and extent of lipolysis in comparison with the pure solid lipid, depending on the lipid loading levels and the morphology. The highest lipid digestion was observed when silica-S was loaded with 34% (w/w) solid lipid, and differential scanning calorimeter (DSC) analysis confirmed the encapsulation of up to 2% (w/w) non-crystalline LOV in this optimal SSL-S formulation. Drug dissolution under non-digesting intestinal conditions revealed a three- to sixfold increase in dissolution efficiencies when compared to the unformulated drug and a LOV-lipid suspension. Furthermore, the SSL-S provided superior drug solubilization under simulated intestinal digesting condition in comparison with the drug-lipid suspension and drug-loaded silica. Therefore, solid lipid and nanoporous silica provides a synergistic effect on optimizing the solubilization of poorly water-soluble compound and the solid lipid-based porous carrier system provides a promising delivery approach to overcome the oral delivery challenges of poorly water-soluble drugs. PMID:27048207

  14. Nanometer-Scale Water-Soluble Macrocycles from Nanometer-Sized Amino Acids

    PubMed Central

    Gothard, Chris M.

    2009-01-01

    This paper introduces the unnatural amino acids m-Abc2K and o-Abc2K as nanometersized building blocks for the creation of water-soluble macrocycles with well-defined shapes. m-Abc2K and o-Abc2K are homologues of the nanometer-sized amino acid Abc2K, which we recently introduced for the synthesis of water-soluble molecular rods of precise length. [J. Am. Chem. Soc. 2007, 129, 7272]. Abc2K is linear (180°), m-Abc2K creates a 120° angle, and o-Abc2K creates a 60° angle. m-Abc2K and o-Abc2K are derivatives of 3’-amino-[1,1’-biphenyl]-4-carboxylic acid and 2’-amino-[1,1’-biphenyl]-4-carboxylic acid, with two propyloxyammonium side chains for water solubility. m-Abc2K and o-Abc2K are prepared as Fmoc-protected derivatives Fmoc-m-Abc2K(Boc)-OH (1a) and Fmoc-o-Abc2K(Boc)-OH (1b). These derivatives can be used alone or in conjunction with Fmoc-Abc2K(Boc)-OH (1c) as ordinary amino acids in Fmoc-based solid-phase peptide synthesis. Building blocks 1a–c were used to synthesize macrocyclic “triangles” 9a–c, “parallelograms” 10a,b, and hexagonal “rings” 11a–d. The macrocycles range from a trimer to a dodecamer, with ring sizes from 24 to 114 atoms, and are 1–4 nm in size. Molecular modeling studies suggest that all the macrocycles except 10b should have well-defined triangle, parallelogram, and ring shapes if all of the amide linkages are trans and the ortho-alkoxy substituents are intramolecularly hydrogen bonded to the amide NH groups. The macrocycles have good water solubility and are readily characterized by standard analytical techniques, such as RP-HPLC, ESI-MS, and NMR spectroscopy. 1H and 13C NMR studies suggest that the macrocycles adopt conformations with all trans-amide linkages in CD3OD, that the “triangles” and “parallelograms” maintain these conformations in D2O, and that the “rings” collapse to form conformations with cis-amide linkages in D2O. PMID:20020731

  15. C-106 High-Level Waste Solids: Washing/Leaching and Solubility Versus Temperature Studies

    SciTech Connect

    GJ Lumetta; DJ Bates; PK Berry; JP Bramson; LP Darnell; OT Farmer III; LR Greenwood; FV Hoopes; RC Lettau; GF Piepel; CZ Soderquist; MJ Steele; RT Steele; MW Urie; JJ Wagner

    2000-01-26

    This report describes the results of a test conducted by Battelle to assess the effects of inhibited water washing and caustic leaching on the composition of the Hanford tank C-106 high-level waste (HLW) solids. The objective of this work was to determine the composition of the C-106 solids remaining after washing with 0.01M NaOH or leaching with 3M NaOH. Another objective of this test was to determine the solubility of various C-106 components as a function of temperature. The work was conducted according to test plan BNFL-TP-29953-8,Rev. 0, Determination of the Solubility of HLW Sludge Solids. The test went according to plan, with only minor deviations from the test plan. The deviations from the test plan are discussed in the experimental section.

  16. Small acid soluble proteins for rapid spore identification.

    SciTech Connect

    Branda, Steven S.; Lane, Todd W.; VanderNoot, Victoria A.; Jokerst, Amanda S.

    2006-12-01

    This one year LDRD addressed the problem of rapid characterization of bacterial spores such as those from the genus Bacillus, the group that contains pathogenic spores such as B. anthracis. In this effort we addressed the feasibility of using a proteomics based approach to spore characterization using a subset of conserved spore proteins known as the small acid soluble proteins or SASPs. We proposed developing techniques that built on our previous expertise in microseparations to rapidly characterize or identify spores. An alternative SASP extraction method was developed that was amenable to both the subsequent fluorescent labeling required for laser-induced fluorescence detection and the low ionic strength requirements for isoelectric focusing. For the microseparations, both capillary isoelectric focusing and chip gel electrophoresis were employed. A variety of methods were evaluated to improve the molecular weight resolution for the SASPs, which are in a molecular weight range that is not well resolved by the current methods. Isoelectric focusing was optimized and employed to resolve the SASPs using UV absorbance detection. Proteomic signatures of native wild type Bacillus spores and clones genetically engineered to produce altered SASP patterns were assessed by slab gel electrophoresis, capillary isoelectric focusing with absorbance detection as well as microchip based gel electrophoresis employing sensitive laser-induced fluorescence detection.

  17. A solid form of ambazone with lactic acid

    NASA Astrophysics Data System (ADS)

    Borodi, Gh.; Muresan-Pop, M.; Kacsó, I.; Bratu, I.

    2012-02-01

    In recent years, much research has been carried out on the preparation of pharmaceutical solid forms due to their improved physical-chemical parameters such as solubility, dissolution rate of the drug, chemical stability, melting point and hygroscopic parameter. The aim of this study was to obtain and to investigate the structural properties of the ambazone (AMB) with lactic acid (LA) solid form. The solid form was obtained starting from the mixture of ambazone with lactic acid (1:1), by grinding method at constant temperature. The obtained compound was investigated via X-ray powder diffraction (PXRD), thermal analysis (DSC, TG-DTA) and infrared (FTIR) spectroscopy. The difference between the patterns of AMB•LA and of the starting compounds evidenced a new compound. Using X-ray powder diffraction method, by indexing procedure the unit cell and the lattice parameters were determined. Thermal and FTIR measurements on the pure compounds and on the (1:1) ground mixture of AMB with LA confirm the new salt form formation.

  18. Crystallization of solid-state materials via decomplexation of soluble complexes

    SciTech Connect

    Doxsee, K.M.

    1998-10-01

    A variety of compounds which are at best sparingly soluble in aqueous media may be readily brought into solution through the formation of soluble coordination complexes. Modification of experimental conditions through, e.g., dilution or slow removal of the complexing agent, leads to supersaturation and, consequently, crystallization of the original solid-state phase. This technique of decomplexation crystallization, both of simple inorganic coordination complexes and of complexes with macrocyclic organic chelating agents, offers the opportunity both to effect the recrystallization of sparingly soluble species and to modify their crystal morphology. Similarly, precursors for solid-state materials may be solubilized in nonaqueous solvents through the formation of soluble complexes and then allowed to undergo reaction crystallization, allowing the examination of both solvent effects and chelation effects on the morphology and phase of the resulting solid-state materials. These effects are often dramatic, and such complexation-mediated crystallization approaches offer promise for the facile preparation of metastable phases from simple precursors under ambient conditions.

  19. A method for rapid liquid-solid phase solubility measurements using the protein lysozyme

    NASA Technical Reports Server (NTRS)

    Pusey, Marc L.; Gernert, Kim

    1988-01-01

    Using hen's egg white lysozyme crystals as the test material, a simple system was developed for rapidly and unambiguously determining solubilities in (aqueous) solutions. The system is based upon a maximization of the solid surface area available for solute transfer to or from the solution, and a minimization of both the solution volume which must be equilibrated and the distance over which diffusive solute exchange occurs. This technique is further enhanced by using duplicate test systems which differ only in that one approaches equilibrium from an oversaturated solution, while the other from an undersaturated solution. Thus, the resulting data pair brackets the solubility value. In practical terms, the data points are found to usually be within 3 percent of each other, and individual solubility data points may usually be made at this resolution within 8-24 h depending upon the temperature change made since the previous determination.

  20. Solubility of small-chain carboxylic acids in supercritical carbon dioxide

    SciTech Connect

    Sparks, Darrell L.; Estevez, L. Antonio; Hernandez, Rafael; McEwen, Jason; French, Todd

    2010-07-08

    The solubility of heptanoic acid and octanoic acid in supercritical carbon dioxide has been determined at temperatures of (313.15, 323.15, and 333.15) K over a pressure range of (8.5 to 30.0) MPa, depending upon the solute. The solubility of heptanoic acid ranged from a solute concentration of (0.08 ± 0.03) kg • m-3 (T = 323.15 K, p = 8.5 MPa) to (147 ± 0.2) kg • m-3 (T = 323.15 K, p = 20.0 MPa). The lowest octanoic acid solubility obtained was a solute concentration of (0.40 ± 0.1) kg • m-3 (T = 333.15 K, p = 10.0 MPa), while the highest solute concentration was (151 ± 2) kg • m-3 (T = 333.15 K, p = 26.7 MPa). In addition, solubility experiments were performed for nonanoic acid in supercritical carbon dioxide at 323.15 K and pressures of (10.0 to 30.0) MPa to add to the solubility data previously published by the authors. In general, carboxylic acid solubility increased with increasing solvent density. The results also showed that the solubility of the solutes decreased with increasing molar mass at constant supercritical-fluid density. Additionally, the efficacy of Chrastil's equation and other density-based models was evaluated for each fatty acid.

  1. Solubility of small-chain carboxylic acids in supercritical carbon dioxide

    DOE PAGESBeta

    Sparks, Darrell L.; Estevez, L. Antonio; Hernandez, Rafael; McEwen, Jason; French, Todd

    2010-07-08

    The solubility of heptanoic acid and octanoic acid in supercritical carbon dioxide has been determined at temperatures of (313.15, 323.15, and 333.15) K over a pressure range of (8.5 to 30.0) MPa, depending upon the solute. The solubility of heptanoic acid ranged from a solute concentration of (0.08 ± 0.03) kg • m-3 (T = 323.15 K, p = 8.5 MPa) to (147 ± 0.2) kg • m-3 (T = 323.15 K, p = 20.0 MPa). The lowest octanoic acid solubility obtained was a solute concentration of (0.40 ± 0.1) kg • m-3 (T = 333.15 K, p = 10.0more » MPa), while the highest solute concentration was (151 ± 2) kg • m-3 (T = 333.15 K, p = 26.7 MPa). In addition, solubility experiments were performed for nonanoic acid in supercritical carbon dioxide at 323.15 K and pressures of (10.0 to 30.0) MPa to add to the solubility data previously published by the authors. In general, carboxylic acid solubility increased with increasing solvent density. The results also showed that the solubility of the solutes decreased with increasing molar mass at constant supercritical-fluid density. Additionally, the efficacy of Chrastil's equation and other density-based models was evaluated for each fatty acid.« less

  2. Solid dispersion as an approach for bioavailability enhancement of poorly water-soluble drug ritonavir.

    PubMed

    Sinha, Shilpi; Ali, Mushir; Baboota, Sanjula; Ahuja, Alka; Kumar, Anil; Ali, Javed

    2010-06-01

    Ritonavir is an antiretroviral drug characterized by low solubility and high permeability which corresponds to BCS class II drug. The purpose of the study was to develop solid dispersion by different methods and investigate them for in vitro and in vivo performance for enhancing dissolution and bioavailability, respectively. Since the drug possesses food-related absorption, the effect of biorelevant media (FaSSIF and FeSSIF state) on dissolution behavior was also studied. The solid dispersion was prepared using Gelucire as carrier in 1:4 ratio by different methods and were characterized for differential scanning calorimetry (DSC), X-ray diffractometry, scanning electron microscopy, and FT-IR. Oral bioavailability of 10 mg of ritonavir in solid dispersion prepared by solvent evaporation (SE1) and melt method (MM1) was compared with pure drug after oral administration of solid dispersion and pure drug to Albino Wistar rats of either sex. The results suggested formation of eutectic solid dispersion. In vitro dissolution studies was performed in 0.1 N HCl and biorelevant media showed enhanced dissolution rate as compared to pure drug in both FeSSIF media and 0.1 N HCl. The apparent rate of absorption of ritonavir from SE1 (C(max) 20221.37 ng/ml, t(max) 0.5 h) was higher than that of MM1 (C(max) 2,462.2, t(max) 1 h) and pure drug (C(max) 1,354.8 ng/ml, t(max) 0.5 h). On the basis of the result obtained, it was concluded that solid dispersion is a good approach to enhance solubility and bioavailability of poorly water-soluble ritonavir. PMID:20238187

  3. Improvement of solubility and dissolution properties of clotrimazole by solid dispersions and inclusion complexes.

    PubMed

    Balata, Gehan; Mahdi, M; Bakera, Rania Abu

    2011-09-01

    Solid dispersions of a slightly water-soluble drug, clotrimazole, were prepared in different weight ratios using polyethyleneglycol 4000 and different molecular weight polyvinyl pyrrolidones as carriers. Moreover, binary and ternary β-cyclodextrin complexes were prepared in different molar ratios. Both solid dispersions and β-cyclodextrin complexes were prepared by solvent evaporation technique. A phase solubility method was used to evaluate the effect of the tested carriers on the aqueous solubility of clotrimazole. The dissolution of all the preparations was tested using the USP paddle method. The selected solid dispersions and inclusion complexes were characterized by differential scanning calorimetry and X-ray powder diffractometry studies, and results clarified the role of the tested carriers in decreasing the crystallinity of clotrimazole and complexing abilities. Based on physical characters and in vitro drug release pattern, polyvinylpyrrolidone solid dispersions (1:1 weight ratio) and ternary cyclodextrin complexes (clotrimazole-β-cyclodextrin complexes with either polymer, 1:1 molar ratio) were selected as ideal batches for suppositories. Suppocire AM/50 mg carbopol 940, was chosen as a suppository base and the suppositories were prepared by molding technique. The prepared suppositories were characterized for weight variation, softening time and drug content. All these properties were found to be ideal. The in vitro drug release pattern was determined in citrate buffer (pH 4.5) containing 1% sodium lauryl sulfate. The in vitro release of clotrimazole from its solid dispersions and inclusion complexes incorporated suppositories was markedly improved when compared to the intact drug incorporated suppositories. Polyvinyl pyrrolidone solid dispersions incorporated suppositories were found to possess excellent antifungal activity. PMID:22923864

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

    NASA Astrophysics Data System (ADS)

    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.

  5. A review of experimental methods for solid solubility determination in cryogenic systems

    NASA Astrophysics Data System (ADS)

    De Stefani, V.; Baba-Ahmed, A.; Richon, D.

    2004-09-01

    Over the past years, there have been a number of serious explosions in air industry, which have resulted in workers injuries and fatalities. At the same time, there has been an increase in the use of air separation products for industrial activities. The quality of air entering an air separation plant is of crucial importance for its safe and reliable operation and the interest in the solubility data of solids in cryogenic liquid solvents is closely connected to the problem of impurities accumulation in the process plant and storage tanks. Such accumulations, especially in liquid oxygen, may cause fouling and blockage in heat exchangers and pipelines and they may eventually cause serious explosions. For this reason the air contaminants composition in liquid oxygen must be determined with great precision. This paper aims at reviewing experimental methods for determining the solubility of solid compounds that may be present in the cryogenic liquefaction processing of air distillation. A review of the literature data on solubility of solids in liquid oxygen and nitrogen is included as well. Emphasis is given to the difficulties in setting-up measuring apparatuses working at extreme conditions, i.e. low compositions and low temperatures.

  6. Determination of soluble solids content in apple products by terahertz time-domain spectroscopy

    NASA Astrophysics Data System (ADS)

    Hao, Guohui; Liu, Jianjun; Hong, Zhi

    2011-08-01

    Soluble solids content is an important index for fruit quality. One of the traditional methods in determining soluble solids content of fruits is refractometry which measures the refractive index in visible or near infrared. Here we reported the use of terahertz time-domain transmission spectroscopy (THz-TDTS) technique for the determination of soluble solids content in apple products. Not only the refractive index, but also the absorption coefficient is used in regression model. In method one, sucrose solutions were for the calibration set , root mean square of validation set (RMSEP) was 0.168% for absorption coefficient model, 0.741% for refractive index model. In method two, apple products were for the calibration set, RMSEP was 0.143% for absorption coefficient model, 0.648% for refractive index model. Less absolute error of 0.2% between predicted and refractometer value has been both obtained from two methods with absorption coefficient model. This result proved the THz-TDS technique is quite potential for nondestructive detection on food quality.

  7. Manganese ore tailing: optimization of acid leaching conditions and recovery of soluble manganese.

    PubMed

    Santos, Olívia de Souza Heleno; Carvalho, Cornélio de Freitas; Silva, Gilmare Antônia da; Santos, Cláudio Gouvêa Dos

    2015-01-01

    Manganese recovery from industrial ore processing waste by means of leaching with sulfuric acid was the objective of this study. Experimental conditions were optimized by multivariate experimental design approaches. In order to study the factors affecting leaching, a screening step was used involving a full factorial design with central point for three variables in two levels (2(3)). The three variables studied were leaching time, concentration of sulfuric acid and sample amount. The three factors screened were shown to be relevant and therefore a Doehlert design was applied to determine the best working conditions for leaching and to build the response surface. By applying the best leaching conditions, the concentrations of 12.80 and 13.64 %w/w of manganese for the global sample and for the fraction -44 + 37 μm, respectively, were found. Microbeads of chitosan were tested for removal of leachate acidity and recovering of soluble manganese. Manganese recovery from the leachate was 95.4%. Upon drying the leachate, a solid containing mostly manganese sulfate was obtained, showing that the proposed optimized method is efficient for manganese recovery from ore tailings. PMID:25284800

  8. Analysis of hyperspectral scattering profiles using a generalized Gaussian distribution function for prediction of apple firmness and soluble solids content

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Hyperspectral scattering provides an effective means for characterizing light scattering in the fruit and is thus promising for noninvasive assessment of apple firmness and soluble solids content (SSC). A critical problem encountered in application of hyperspectral scattering technology is analyzing...

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

    PubMed Central

    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

  10. Structure-property relationships in halogenbenzoic acids: Thermodynamics of sublimation, fusion, vaporization and solubility.

    PubMed

    Zherikova, Kseniya V; Svetlov, Aleksey A; Kuratieva, Natalia V; Verevkin, Sergey P

    2016-10-01

    Temperature dependences of vapor pressures for 2-, 3-, and 4-bromobenzoic acid, as well as for five isomeric bromo-methylbenzoic acids were studied by the transpiration method. Melting temperatures and enthalpies of fusion for all isomeric bromo-methylbenzoic acids and 4-bromobenzoic acid were measured with a DSC. The molar enthalpies of sublimation and vaporization were derived. These data together with results available in the literature were collected and checked for internal consistency using a group-additivity procedure and results from X-ray structural diffraction studies. Specific (hydrogen bonding) interactions in the liquid and in the crystal phase of halogenbenzoic acids were quantified based on experimental values of vaporization and sublimation enthalpies. Structure-property correlations of solubilities of halogenobenzoic acids with sublimation pressures and sublimation enthalpies were developed and solubilities of bromo-benzoic acids were estimated. These new results resolve much of the ambiguity in the available thermochemical and solubility data on bromobenzoic acids. The approach based on structure property correlations can be applied for the assessment of water solubility of sparingly soluble drugs. PMID:27424058

  11. Separation of asphaltic materials from heptane soluble components in liquified solid hydrocarbonaceous extracts

    SciTech Connect

    Gleim, W.

    1980-07-08

    An improved method is described for maximizing the separation of the heat labile fraction of asphaltic materials in a liquified solid hydrocarbonaceous extract, which comprises the steps of: (A) adding a solvent having a boiling range of from about 50 to 200/sup 0/C for the heptane solubles of said extract, (B) effecting a mixing of said solvent and said extract and providing a pressurized centrifuging action of the combined stream in a confined pressure-tight powered centrifuging zone at a temperature in the range of 100/sup 0/C, to about 200/sup 0//c while at an elevated pressure at least sufficient to maintain the solvent material in a liquid state, whereby to separate the heavier heat labile asphaltic materials fraction from the mixture, and (C) effecting the withdrawal of the asphaltic fraction from the centrifuging zone substantially free of the resulting solution of the heptane soluble liquified fuel extract.

  12. Solid solubility, phase transitions, thermal expansion, and compressibility in Sc1-xAlxF3

    NASA Astrophysics Data System (ADS)

    Morelock, Cody R.; Gallington, Leighanne C.; Wilkinson, Angus P.

    2015-02-01

    With the goal of thermal expansion control, the synthesis and properties of Sc1-xAlxF3 were investigated. The solubility limit of AlF3 in ScF3 at ~1340 K is ~50%. Solid solutions (x≤0.50) were characterized by synchrotron powder diffraction at ambient pressure between 100 and 900 K and at pressures <0.414 GPa while heating from 298 to 523 K. A phase transition from cubic to rhombohedral is observed. The transition temperature increases smoothly with Al3+ content, approaching 500 K at the solid solubility limit, and also upon compression at fixed Al3+ content. The slope of the pressure-temperature phase boundary is ~0.5 K MPa-1, which is steep relative to that for most symmetry-lowering phase transitions in perovskites. The volume coefficient of thermal expansion (CTE) for the rhombohedral phase is strongly positive, but the cubic-phase CTE varies from negative (x<0.15) to near-zero (x=0.15) to positive (x>0.20) between ~600 and 800 K. The cubic solid solutions elastically stiffen on heating, while Al3+ substitution causes softening at a given temperature.

  13. Water solubility enhancement of some organic pollutants and pesticides by dissolved humic and fulvic acids

    USGS Publications Warehouse

    Chiou, C.T.; Malcolm, R.L.; Brinton, T.I.; Kile, D.E.

    1986-01-01

    Water solubility enhancements by dissolved humic and fulvic acids from soil and aquatic origins and by synthetic organic polymers have been determined for selected organic pollutants and pesticides (p,p???-DDT, 2,4,5,2???,5???-PCB, 2,4,4???-PCB, 1,2,3-trichlorobenzene, and lindane). Significant solubility enhancements of relatively water-insoluble solutes by dissolved organic matter (DOM) of soil and aquatic origins may be described in terms of a partition-like interaction of the the solutes with the microscopic organic environment of the high-molecular-weight DOM species; the apparent solute solubilities increase linearly with DOM concentration and show no competitive effect between solutes. With a given DOM sample, the solute partition coefficient (Kdom) increases with a decrease of solute solubility (Sw) or with an increase of the solute's octanol-water partition coefficient (Kow). The Kdom values of solutes with soil-derived humic acid are approximately 4 times greater than with soil fulvic acid and 5-7 times greater than with aquatic humic and fulvic acids. The effectiveness of DOM in enhancing solute solubility appears to be largely controlled by the DOM molecular size and polarity. The relative inability of high-molecular-weight poly(acrylic acids) to enhance solute solubility is attributed to their high polarities and extended chain structures that do not permit the formation of a sizable intramolecular nonpolar environment.

  14. Formation of water soluble complexes of ?: solid-state reaction between tertiary amines and ?

    NASA Astrophysics Data System (ADS)

    Mohan, H.; Priyadarsini, K. I.; Tyagi, A. K.; Mittal, J. P.

    1996-11-01

    Water soluble complexes of 0953-4075/29/21/015/img3 have been prepared on solid-state mechano-chemical reaction between 0953-4075/29/21/015/img3 and tertiary amines (hexamine, DABCO) at room temperature 0953-4075/29/21/015/img5. The product is characterized by x-ray diffraction and FTIR methods. It is presumably due to the charge transfer interactions between electron affinic 0953-4075/29/21/015/img3 and electron rich tertiary amines.

  15. Influence of solid state fermentation by Trichoderma spp. on solubility, phenolic content, antioxidant, and antimicrobial activities of commercial turmeric.

    PubMed

    Mohamed, Saleh A; Saleh, Rashad M; Kabli, Saleh A; Al-Garni, Saleh M

    2016-05-01

    The influence of solid state fermentation (SSF) by Trichoderma spp. on the solubility, total phenolic content, antioxidant, and antibacterial activities of turmeric was determined and compared with unfermented turmeric. The solubility of turmeric was monitored by increase in its phenolic content. The total phenolic content of turmeric extracted by 80% methanol and water after SSF by six species of Trichoderma spp. increased significantly from 2.5 to 11.3-23.3 and from 0.5 to 13.5-20.4 GAE/g DW, respectively. The antioxidant activities of fermented turmeric were enhanced using 2,2-diphenyl-1-picrylhydrazyl (DPPH), 2,2'-azino-bis (3-ethylbenzo-thiazoline-6-sulfonic acid) (ABTS), and ferric ion-reducing antioxidant power (FRAP) assays. The antibacterial activity of fermented turmeric against human-pathogenic bacteria Escherichia coli, Streptococcus agalactiae, Staphylococcus aureus, Entreococcus faecalis, Methicillin-Resistant S. aureus, Klebsiella pneumonia, and Pseudomonas aeruginosae showed a broad spectrum inhibitory effect. In conclusion, the results indicated the potentials of using fermented turmeric as natural antioxidant and antimicrobial material for food applications. PMID:27023794

  16. Thermodynamics and solubility of (UxNp1-x) O2(am) solid solution in the carbonate system

    SciTech Connect

    Rai, Dhanpat; Hess, Nancy J.; Yui, Mikazu; Felmy, Andrew R.; Moore, D. A.

    2004-12-31

    SUMMARY-The formation of a solid solution can significantly affect the solubility of a minor component. The objectives of this study were to determine the nature of U(IV) and Np(IV) solid solutions and their thermodynamic properties. For this purpose...

  17. SUPERCRITICAL CARBON DIOXIDE-SOLUBLE LIGANDS FOR EXTRACTING ACTINIDE METAL IONS FROM POROUS SOLIDS

    EPA Science Inventory

    The objective of this project is to develop novel, substituted diphosphonic acid ligands that can be used for supercritical carbon dioxide extraction (SCDE) of actinide ions from solid wastes. These ligands will be used to investigate fundamental aspects of metal extraction into...

  18. Overlapping solid solubility in mechanically alloyed Fe-Ni and Fe-Cu

    NASA Astrophysics Data System (ADS)

    Schilling, P. J.; Palshin, V.; Tittsworth, R. C.; He, J. H.; Ma, E.

    2003-12-01

    Solid solutions formed by mechanical alloying in the negative heat of mixing Fe-Ni system and the positive heat of mixing Fe-Cu system were studied. X-ray absorption near edge structure (XANES) spectroscopy data were analyzed to obtain the phase fractions and phase compositions for various overall compositions across the bcc/fcc two-phase region. For both systems, at each nominal composition of the powder mixture, the two solutions formed both have the same composition as the overall alloy. It is concluded that the two-phase coexistence represents an extended region of overlapping solubility for the two phases, rather than the usual two-phase region or a clear switchover at the concentration where the two phases have the same free energy. In terms of these features, the two binary systems, one with negative heat of mixing and one with positive heat of mixing, behave the same way. The external forcing action of mechanical alloying at low temperatures drives the system toward composition homogenization. There is no stable or metastable equilibrium, and the common tangent construction and lever rule are not applicable. What results is a novel two-phase coexistence which is defined by a region of overlapping solubility, rather than the normal solubility gap. That there can be two polymorphs at each composition even after the long ball-milling treatment represents a new type of steady-state two-phase coexistence that is completely different from the normal two-phase region dictated by thermodynamics.

  19. Solid-state actinide acid phosphites from phosphorous acid melts

    NASA Astrophysics Data System (ADS)

    Oh, George N.; Burns, Peter C.

    2014-07-01

    The reaction of UO3 and H3PO3 at 100 °C and subsequent reaction with dimethylformamide (DMF) produces crystals of the compound (NH2(CH3)2)[UO2(HPO2OH)(HPO3)]. This compound crystallizes in space group P21/n and consists of layers of uranyl pentagonal bipyramids that share equatorial vertices with phosphite units, separated by dimethylammonium. In contrast, the reaction of phosphorous acid and actinide oxides at 210 °C produces a viscous syrup. Subsequent dilution in solvents and use of standard solution-state methods results in the crystallization of two polymorphs of the actinide acid phosphites An(HPO2OH)4 (An=U, Th) and of the mixed acid phosphite-phosphite U(HPO3)(HPO2OH)2(H2O)·2(H2O). α- and β-An(HPO2OH)4 crystallize in space groups C2/c and P21/n, respectively, and comprise a three-dimensional network of An4+ cations in square antiprismatic coordination corner-sharing with protonated phosphite units, whereas U(HPO3)(HPO2OH)2(H2O)2·(H2O) crystallizes in a layered structure in space group Pbca that is composed of An4+ cations in square antiprismatic coordination corner-sharing with protonated phosphites and water ligands. We discuss our findings in using solid inorganic reagents to produce a solution-workable precursor from which solid-state compounds can be crystallized.

  20. Carbon-based strong solid acid for cornstarch hydrolysis

    SciTech Connect

    Nata, Iryanti Fatyasari; Irawan, Chairul; Mardina, Primata; Lee, Cheng-Kang

    2015-10-15

    Highly sulfonated carbonaceous spheres with diameter of 100–500 nm can be generated by hydrothermal carbonization of glucose in the presence of hydroxyethylsulfonic acid and acrylic acid at 180 °C for 4 h. The acidity of the prepared carbonaceous sphere C4-SO{sub 3}H can reach 2.10 mmol/g. It was used as a solid acid catalyst for the hydrolysis of cornstarch. Total reducing sugar (TRS) concentration of 19.91 mg/mL could be obtained by hydrolyzing 20 mg/mL cornstarch at 150 °C for 6 h using C4-SO{sub 3}H as solid acid catalyst. The solid acid catalyst demonstrated good stability that only 9% decrease in TRS concentration was observed after five repeat uses. The as-prepared carbon-based solid acid catalyst can be an environmentally benign replacement for homogeneous catalyst. - Highlights: • Carbon solid acid was successfully prepared by one-step hydrothermal carbonization. • The acrylic acid as monomer was effectively reduce the diameter size of particle. • The solid acid catalyst show good catalytic performance of starch hydrolysis. • The solid acid catalyst is not significantly deteriorated after repeated use.

  1. Experimental determination and prediction of (solid+liquid) phase equilibria for binary mixtures of heavy alkanes and fatty acids

    NASA Astrophysics Data System (ADS)

    Benziane, Mokhtar; Khimeche, Kamel; Dahmani, Abdellah; Nezar, Sawsen; Trache, Djalal

    2012-06-01

    Solid-liquid equilibria for three binary mixtures, n-Eicosane (1) + Lauric acid (2), n-Tetracosane (1) + Stearic acid (2), and n-Octacosane (1) + Palmitic acid (2), were measured using a differential scanning calorimeter. Simple eutectic behaviour was observed for these systems. The experimental results were correlated by means of the modified UNIFAC (Larsen and Gmehling versions), UNIQUAC and ideal models. The root-mean-square deviations of the solubility temperatures for all measured data vary from 0.26 to 3.15 K and depend on the particular model used. The best solubility correlation was obtained with the UNIQUAC model.

  2. Carbon-based strong solid acid for cornstarch hydrolysis

    NASA Astrophysics Data System (ADS)

    Nata, Iryanti Fatyasari; Irawan, Chairul; Mardina, Primata; Lee, Cheng-Kang

    2015-10-01

    Highly sulfonated carbonaceous spheres with diameter of 100-500 nm can be generated by hydrothermal carbonization of glucose in the presence of hydroxyethylsulfonic acid and acrylic acid at 180 °C for 4 h. The acidity of the prepared carbonaceous sphere C4-SO3H can reach 2.10 mmol/g. It was used as a solid acid catalyst for the hydrolysis of cornstarch. Total reducing sugar (TRS) concentration of 19.91 mg/mL could be obtained by hydrolyzing 20 mg/mL cornstarch at 150 °C for 6 h using C4-SO3H as solid acid catalyst. The solid acid catalyst demonstrated good stability that only 9% decrease in TRS concentration was observed after five repeat uses. The as-prepared carbon-based solid acid catalyst can be an environmentally benign replacement for homogeneous catalyst.

  3. IUPAC-NIST Solubility Data Series. 90. Hydroxybenzoic Acid Derivatives in Binary, Ternary, and Multicomponent Systems. Part I. Hydroxybenzoic Acids, Hydroxybenzoates, and Hydroxybenzoic Acid Salts in Water and Aqueous Systems

    NASA Astrophysics Data System (ADS)

    Goto, Rensuke; Fukuda, Hiroshi; Königsberger, Erich; Königsberger, Lan-Chi

    2011-03-01

    The solubility data for well-defined binary, ternary, and multicomponent systems of solid-liquid type are reviewed. One component, which is 2-, 3-, and 4-hydroxybenzoic acids, 4-hydroxybenzoate alkyl esters (parabens), or hydroxybenzoic acid salts, is in the solid state at room temperature and another component is liquid water, meaning that all of the systems are aqueous solutions. The ternary or multicomponent systems include organic substances of various classes (hydrocarbons of several structural types, halogenated hydrocarbons, alcohols, acids, ethers, esters, amides, and surfactants) or inorganic substances. Systems reported in the primary literature from 1898 through 2000 are compiled. For seven systems, sufficient binary data for hydroxybenzoic acids or parabens in water are available to allow critical evaluation. Almost all data are expressed as mass and mole fractions as well as the originally reported units, while some data are expressed as molar concentration.

  4. Synthesis and solubility of Pb-Ca and P-As hydroxylapatite solid solutions

    NASA Astrophysics Data System (ADS)

    Puzio, Bartosz; Młynarska, Maria; Motyka, Joanna; Oknińska, Joanna; Mandelt, Agnieszka; Chlebowska, Patrycja; Kwaśniak-Kominek, Monika; Manecki, Maciej

    2016-04-01

    The objective of the study are three solid solution series: - HPY hydroxylpyromorphite Pb5(PO4)3OH - HAP hydroxylapatite Ca5(PO4)3OH - HAP hydroxylapatite Ca5(PO4)3OH - JBM johnbaumite Ca5(AsO4)3OH - JBM johnbaumite Ca5(AsO4)3OH - HMI hydroxylmimetite Pb5(AsO4)3OH The phases were synthesized from aqueous solutions at high pH (over 8) at ambient temperature by dropwise mixing of chemical reagents: Pb(NO3)2, Ca(NO3)2.4H2O, (NH4)H2PO4, and Na2AsHO4.7H2O. The products of all syntheses are crystalline, monomineral fine powders (crystal size less than 1 μm). Their chemical composition is close to theoretical. Systematic shift of XRD peaks and FTIR or Raman bands is observed within the solid solution series. Dissolution experiments were run at 5oC, 25oC, 45oC, and 65oC. An aliquot of 0.5g of each phase was dissolved in 250 mL of 0.05M NH4NO3 (pH between 3 and 5) for about 3 months. In all cases dissolution resulted in increase of pH by about 1. The systems were considered in equilibrium when three consecutive samplings (ca. two weeks apart) resulted in similar concentrations (within 3 standard deviations). The dissolution of all phases in question is incongruent. The amount of precipitating secondary phases was too small for identification. The results of HPY - HAP dissolution experiments are inconclusive due to strongly incongruent dissolution. This is partially in contrary to recent report by Zhu et al. (2015). Systematic increase of solubility is observed in HAP - JBM series. Also, the solubility of these phases increases with the increase of temperature. This is more pronounced for HAP than for JBM. Systematic increase of solubility is also observed in HMI - JBM series. This work is partially funded by AGH research grant no 11.11.140.319 and partially by Polish NCN grant No 2014/01/M/ST10/00355. Zhu,Y., Zhu, Z., Zhao, X., Liang, Y., Huang, Y., 2015. Characterization, dissolution, and solubility of lead hydroxypyromorphite Pb5(PO4)3OH at 25-45oC. Journal of Chemistry

  5. THERMODYNAMICS AND SOLUBILITY OF (UxNp1-x)O2(am) SOLID SOLUTION IN THE CARBONATE SYSTEM

    SciTech Connect

    Rai, Dhanpat; Hess, Nancy J.; Yui, Mikazu; Felmy, Andrew R.; Moore, Dean A.

    2004-03-15

    ABSTRACT -The formation of a solid solution can significantly affect the solubility of a minor component. The objectives of this study were to determine the nature of U(IV) and Np(IV) solid solutions and their thermodynamic properties. For this purpose, co-precipitates of U(IV) and Np(IV) [(UxNp1-x )O2(am), with values for x of 0.95, 0.85, 0.50, 0.15, and 0.05] were prepared, characterized, and used to determine their solubility as a function of K2CO3 concentrations ranging from 1.0 m to 5.0 m in the presence of 0.01 m Na2S2O4 and 0.01 m KOH, and as a function of KHCO3 concentrations ranging from 0.1 m to 0.8 m in the presence of 0.01 m Na2S2O4. The solubility data show that the equilibrium in these systems is reached in <7 days, the solubility-controlling solids are amorphous, and that we were successful in maintaining U and Np in the tetravalent state. A scanning electron microscope equipped with energy dispersive spectrometry and x-ray absorption spectroscopic analyses of the solids indicated the equilibrated co-precipitates to be solid solutions. A close agreement between the thermodynamic predictions, assuming an ideal solid solution, and the experimental solubilities shows that U(IV) and Np(IV) form an ideal solid solution and that non-ideal solid solution behavior for this system can be ruled out.

  6. Solubility of HOBr in Acidic Solution and Implications for Liberation of Halogens Via Aerosol Processing

    NASA Technical Reports Server (NTRS)

    Iraci, Laura T.; Michelsen, R. R.; Rammer, T. A.; Ashbourn, S. F. M.

    2004-01-01

    Halogen species are known to catalytically destroy ozone in several regions of the atmosphere. In addition to direct catalytic losses, bromine compounds can indirectly enhance ozone loss through coupling to other radical families. Hypobromous acid (HOBr) is a key species in the linkage of BrOx to ClOx and HOx. The aqueous- phase coupling reaction HOBr + HCI (right arrow) BrCl + H2O may provide a pathway for chlorine activation on sulfate aerosols at temperatures warmer than those required for polar stratospheric cloud formation. We have measured t h e solubility of HOBr in 45 - 70 wt% sulfuric acid solutions. Over the temperature range 201 - 252 K, HOBr is quite soluble in sulfuric acid, H* = 10(exp 4) - 10(exp 7) mol dm(exp -3) atm(exp -1). The expected inverse dependence of H* on temperature was observed, but only a weak dependence on acidity was found. The solubility of HOBr is comparable to that of HBr, indicating that equilibrium concentrations of HOBr could equal or exceed those of HBr in upper tropospheric and lower stratospheric aerosols. Despite the high solubility of HOBr, aerosol volumes are not large enough to sequester a significant fraction of inorganic bromine from the gas phase. Our measurements of HOBr uptake in aqueous sulfuric acid in the presence of other brominated gases show the evolution of gaseous products including Br2O and Br2.

  7. Synthesis of water soluble glycosides of pentacyclic dihydroxytriterpene carboxylic acids as inhibitors of α-glucosidase.

    PubMed

    Xu, Jiancong; Nie, Xuliang; Hong, Yanping; Jiang, Yan; Wu, Guoqiang; Yin, Xiaoli; Wang, Chunrong; Wang, Xiaoqiang

    2016-04-01

    A series of compounds were synthesized by glycosylation of maslinic acid (MA) and corosolic acid (CA) with monosaccharides and disaccharides, and the structures of the derivatives were elucidated by standard spectroscopic methods including (1)H NMR, (13)C NMR and HRMS. The α-glucosidase inhibitory activities of all the novel compounds were evaluated in vitro. The solubility and inhibitory activity of α-glucosidase assays showed that the bis-disaccharide glycosides of triterpene acids possessed higher water solubility and α-glucosidase inhibitory activities than the bis-monosaccharide glycosides. Among these compounds, maslinic acid bis-lactoside (8e, IC50 = 684 µM) and corosolic acid bis-lactoside (9e, IC50 = 428 µM) had the best water solubility, and 9e exhibited a better inhibitory activity than acarbose (IC50 = 478 µM). However, most of glycosylated derivatives possessed lower inhibitory activities than the parent compounds, although their water solubility was enhanced obviously. Moreover, the kinetic inhibition studies indicated that 9e was a non-competitive inhibitor, and structure-activity relationships of the derivatives are also discussed. PMID:26974355

  8. Effect of alcohols and neutral salt on the thermal stability of soluble and precipitated acid-soluble collagen

    PubMed Central

    Russell, Allan E.

    1973-01-01

    The effects of mono- and poly-hydric alcohols in the presence of KCl on the intrinsic stability of collagen molecules in dilute acid solution were compared with corresponding solvent and salt effects on the increased stability of the aggregated molecules in salt-precipitated fibrils. Salt addition decreased solubility and increased the thermal stability of fibrils, but progressively decreased the stability of collagen molecules in solution. In contrast, the alcohols enhanced solubility and decreased fibril stability, the effects increasing with solvent hydrocarbon chain length and with decreasing hydroxyl/methylene-group ratio. Molar destabilization of dissolved collagen by alcohols was lower than for fibrils, and at low salt concentration, both ethylene glycol and glycerol were structural stabilizers. Electron-micrograph studies indicated that salt-precipitated fibrils tended to adopt the native aggregation mode, and qualitatively similar solvent effects were observed in insoluble collagens. Implications of the experimental findings are discussed in terms of a model in which electrostatic and apolar interactions mainly govern the excess of stability in collagen fibrils whereas intrinsic stability of single molecules is a function of polar interactions and polypeptide-chain rigidity. PMID:4737319

  9. Water-soluble and solid-state speciation of phosphorus in stabilized sewage sludge.

    PubMed

    Huang, Xiao-Lan; Shenker, Moshe

    2004-01-01

    Three chemicals, ferrous sulfate (Fe-sul), calcium oxide (CaO), and aluminum sulfate (alum), were used to stabilize phosphorus (P) in fresh, anaerobically digested sewage sludge (FSS). The chemically stabilized sludge materials and biosolids compost (BSC) were compared with the FSS with respect to water-soluble phosphorus (WSP) content in its inorganic (WSP(i)) and organic (WSP(o)) forms as well as water-soluble organic carbon (DOC). Solid-state P speciation was further probed by X-ray diffraction (XRD) and scanning electron microscopy (SEM) equipped with energy-dispersive X-ray elemental spectrometry (EDXS). Water-soluble P was effectively controlled by a wide range of Fe-sul or CaO additions to the sludge (Ca to P ratio = 3.47-17.72, Fe to P ratio = 1.01-16.53), but by only a narrow range (Al to P ratio = 1.04-2.87) of alum addition. The WSP content in the BSC was also depressed, but to a lesser extent. The pH in the treated sludge ranged from 3.0 to 12.5 and served as a key factor to control P chemistry. No correlation was observed between DOC and WSP(o). No crystallized Ca-P minerals were detected in the CaO-stabilized sludge, but brushite crystallization seemed to be obtained by low addition of Fe-sul and alum. Variscite and strengite crystallization was obtained following high addition of Fe-sul or alum, as detected by XRD and SEM-EDXS. Adsorption of P by newly formed Fe-hydroxide seems to play an important role in the Fe-sul-stabilized sludge. We concluded that administration of the tested chemicals at the proper rate can effectively reduce the hazard of P release and leaching from sludge. PMID:15356251

  10. Solubility calculations of branched and linear amino acids using lattice cluster theory

    NASA Astrophysics Data System (ADS)

    Fischlschweiger, Michael; Enders, Sabine; Zeiner, Tim

    2014-09-01

    In this work, the activity coefficients and the solubility of amino acids in water were calculated using the lattice cluster theory (LCT) combined with the extended chemical association lattice model allowing self-association as well as cross-association. This permits the study of the influence of the amino acids structure on the thermodynamic properties for the first time. By the used model, the activity coefficient and solubilities of the investigated fourteen amino acids (glycine, alanine, γ-aminobutyric acid, dl-valine, dl-threonine, dl-methionine, l-leucine, l-glutamic acid, l-proline, hydroxyproline, histidine, l-arginine, α-amino valeric acid) could be described in good accordance with experimental data. In the case of different α-amino acids, but different hydrocarbon chains, the same interaction energy parameter can be used within the LCT. All studied amino acids could be modelled using the same parameter for the description of the amino acid association properties. The formed cross-associates contain more amino acids than expressed by the overall mole fraction of the solution. Moreover, the composition of the cross-associates depends on temperature, where the amount of amino acids increases with increasing temperature.

  11. Peculiarities of hydrogen permeation through Zr-1%Nb alloy and evaluation of terminal solid solubility

    NASA Astrophysics Data System (ADS)

    Denisov, E. A.; Kompaniets, M. V.; Kompaniets, T. N.; Bobkova, I. S.

    2016-04-01

    Hydrogen permeation through Zr-1%Nb alloy was studied at the temperature below the temperature of α-β transition. Analysis of the transient permeation curves from a closed volume in a surface limited regime allowed to determine total and mobile hydrogen concentrations. At the mobile hydrogen concentration of 4.3 at% a part of the absorbed hydrogen is cut out of permeation process. Increase of the mobile hydrogen concentration in α-phase of Zr-1%Nb alloy is ceasing at the concentration of (5.5 ± 0.3) at%, which is the maximum possible concentration of the mobile hydrogen in α-phase of the studied alloy. From this moment on all absorbed hydrogen is spent on hydride formation. The obtained results are compared with those obtained by means of traditional techniques for terminal solid solubility determination.

  12. Solid solubility and thermal expansion studies of uranium-europium mixed oxides

    NASA Astrophysics Data System (ADS)

    Venkata Krishnan, R.; Jogeswararao, G.; Panneerselvam, G.; Antony, M. P.; Ananthasivan, K.

    2015-10-01

    Uranium-europium mixed oxides (U1-yEuy)O2-x (y = 0.2, 0.4, 0.6, 0.65, 0.7, 0.75, 0.8) were prepared by citrate gel-combustion synthesis and characterized by using X-ray diffraction (XRD). The terminal solid solubility of EuO1.5 in UO2 is in the composition range 60-65 mol% EuO1.5. The coefficients of thermal expansions at 1973 K for (U1-yEuy)O2-x (y = 0.2, 0.4, 0.6) measured by using high-temperature X-ray diffraction (HTXRD) were found to be 15.80, 14.81 and 14.30 × 10-6 K-1 respectively.

  13. Role of Acid Mobilization in Iron Solubility of Smaller Mineral Dust Aerosols

    NASA Astrophysics Data System (ADS)

    Ito, A.

    2011-12-01

    Iron (Fe) is an essential element for phytoplankton. The majority of iron is transported from arid regions to the open ocean, but is mainly in an insoluble form. Since most aquatic organisms can take up iron only in the dissolved form, the amount of soluble iron is of key importance. Atmospheric processing of mineral aerosols by anthropogenic pollutants may transform insoluble iron into soluble forms. Compared to dust, combustion aerosols often contain iron with higher solubility. This paper discusses the factors that affect the iron solubility in mineral aerosols on a global scale using an aerosol chemistry transport model. Bioavailable iron is derived from atmospheric processing of relatively insoluble iron from desert sources and from direct emissions of soluble iron from combustion sources such as biomass and fossil fuels burning. The iron solubility from onboard cruise measurements over the Atlantic and the Pacific Oceans in 2001 is used to evaluate the model performance in simulating soluble iron. Sensitivity simulations from dust sources with no atmospheric processing by acidic species systematically underestimate the soluble iron concentration in fine particles. Improvement of the agreement between the model results and observations is achieved by the use of a faster iron dissolution rate in fine particles associated with anthropogenic pollutants (e.g., sulphate). Accurate simulation of the abundance of soluble iron in fine aerosols has important implications with regards to ocean fertilization because of the longer residence time of smaller particles, which supply nutrients to more remote ocean biomes. The model reveals a larger deposition of soluble iron for the fine mode than that for the coarse mode in northern oceans due to acid mobilization. The ratio of deposition rate of soluble iron in the fine mode to the total aerosols in the South Atlantic Ocean (40-60%) is less than that in northern oceans (70-100%). These results suggest that Patagonian dust

  14. Physicochemical properties of tadalafil solid dispersions - Impact of polymer on the apparent solubility and dissolution rate of tadalafil.

    PubMed

    Wlodarski, K; Sawicki, W; Haber, K; Knapik, J; Wojnarowska, Z; Paluch, M; Lepek, P; Hawelek, L; Tajber, L

    2015-08-01

    To improve solubility of tadalafil (Td), a poorly soluble drug substance (3μg/ml) belonging to the II class of the Biopharmaceutical Classification System, its six different solid dispersions (1:1, w/w) in the following polymers: HPMC, MC, PVP, PVP-VA, Kollicoat IR and Soluplus were successfully produced by freeze-drying. Scanning electron microscopy showed a morphological structure of solid dispersions typical of lyophilisates. Apparent solubility and intrinsic dissolution rate studies revealed the greatest, a 16-fold, increase in drug solubility (50μg/ml) and a significant, 20-fold, dissolution rate enhancement for the Td/PVP-VA solid dispersion in comparison with crystalline Td. However, the longest duration of the supersaturation state in water (27μg/ml) over 24h was observed for the Td solid dispersion in HPMC. The improved dissolution of Td from Td/PVP-VA was confirmed in the standard dissolution test of capsules filled with solid dispersions. Powder X-ray diffraction and thermal analysis showed the amorphous nature of these binary systems and indicated the existence of dispersion at the molecular level and its supersaturated character, respectively. Nevertheless, as evidenced by film casting, the greatest ability to dissolve Td in polymer was determined for PVP-VA. The crystallization tendency of Td dispersed in Kollicoat IR could be explained by the low Tg (113°C) of the solid dispersion and the highest difference in Hansen solubility parameters (6.8MPa(0.5)) between Td and the polymer, although this relationship was not satisfied for the partially crystalline dispersion in PVP. Similarly, no correlation was found between the strength of hydrogen bonds investigated using infrared spectroscopy and the physical stability of solid dispersions or the level of supersaturation in aqueous solution. PMID:25998701

  15. Effects of CO2 enrichment on soluble amino acids and organic acids in barley primary leaves as a function of age, photoperiod, and chlorosis

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Responses of soluble amino acids and organic acids to CO2 enrichment were determined using barley primary leaves (Hordeum vulgare L. cv. Brant). Plants were grown in controlled environment chambers using either ambient (36 Pa) or elevated (100 Pa) CO2 treatments. Total soluble amino acids were inc...

  16. Hydrocracking with new solid acid catalysts: Model compounds studies

    SciTech Connect

    Sharma, R.K.; Diehl, J.W.; Olson, E.S. )

    1990-01-01

    Two new solid acid catalysts have been prepared by supporting zinc chloride on silica gel and acid-exchanged montmorillonite. The acid properties of these catalysts were determined by Hammett indicator method which showed that highly Bronsted acidic sites were present. SEM/EDS studies indicated a uniform distribution of silicon, zinc, and chlorine in the silica gel-zinc chloride catalyst. The activities of these catalysts in the hydrocracking of bibenzyl, polybenzyl, alkylbenzenes, and other heteroatom substituted aromatics were investigated. Their results with model compounds account for the effectiveness of these solid acid catalysts for conversion of coals to lower molecular weight materials.

  17. Phenolic acids and antioxidant capacity of distillers dried grains with solubles (DDGS) as compared with corn

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Three sets of ground corn and the corresponding distillers dried grains with solubles (DDGS) were collected from three commercial plants and analyzed for individual phenolic acids by high performance liquid chromatography coupled with diode array and/or mass spectrometry and for antioxidant capacity...

  18. Phenolic acids and antioxidant activity of distillers dried grains with solubles (DDGS) as compared with corn

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Sample sets of ground corn and the corresponding distillers dried grains with solubles (DDGS) were collected from three commercial plants in Iowa. Phenolic acids were analyzed by high performance liquid chromatography coupled with diode array and/or mass spectrometry. The antioxidant activity was ...

  19. ALUMINUM SOLUBILITY, CALCIUM-ALUMINUM EXCHANGE, AND PH IN ACID FOREST SOILS

    EPA Science Inventory

    Important components in several models designed to describe the effects of acid deposition on soils and surface waters are the pH-A1 and Ca-A1 exchange relationships. f A1 solubility is controlled by A1 trihydroxide minerals, the theoretical pH-A1 relationship can be described by...

  20. Mefenamic acid taste-masked oral disintegrating tablets with enhanced solubility via molecular interaction produced by hot melt extrusion technology

    PubMed Central

    Alshehri, Sultan M.; Park, Jun-Bom; Alsulays, Bader B.; Tiwari, Roshan V.; Almutairy, Bjad; Alshetaili, Abdullah S.; Morott, Joseph; Shah, Sejal; Kulkarni, Vijay; Majumdar, Soumyajit; Martin, Scott T.; Mishra, Sanjay; Wang, Lijia; Repka, Michael A.

    2015-01-01

    The objective of this study was to enhance the solubility as well as to mask the intensely bitter taste of the poorly soluble drug, Mefenamic acid (MA). The taste masking and solubility of the drug was improved by using Eudragit® E PO in different ratios via hot melt extrusion (HME), solid dispersion technology. Differential scanning calorimetry (DSC) studies demonstrated that MA and E PO were completely miscible up to 40% drug loads. Powder X-ray diffraction analysis indicated that MA was converted to its amorphous phase in all of the formulations. Additionally, FT-IR analysis indicated hydrogen bonding between the drug and the carrier up to 25% of drug loading. SEM images indicated aggregation of MA at over 30% of drug loading. Based on the FT-IR, SEM and dissolution results for the extrudates, two optimized formulations (20% and 25% drug loads) were selected to formulate the orally disintegrating tablets (ODTs). ODTs were successfully prepared with excellent friability and rapid disintegration time in addition to having the desired taste-masking effect. All of the extruded formulations and the ODTs were found to be physically and chemically stable over a period of 6 months at 40°C/75% RH and 12 months at 25°C/60% RH, respectively. PMID:25914727

  1. Determination of water-soluble forms of oxalic and formic acids in soils by ion chromatography

    NASA Astrophysics Data System (ADS)

    Karicheva, E.; Guseva, N.; Kambalina, M.

    2016-03-01

    Carboxylic acids (CA) play an important role in the chemical composition origin of soils and migration of elements. The content of these acids and their salts is one of the important characteristics for agrochemical, ecological, ameliorative and hygienic assessment of soils. The aim of the article is to determine water-soluble forms of same carboxylic acids — (oxalic and formic acids) in soils by ion chromatography with gradient elution. For the separation and determination of water-soluble carboxylic acids we used reagent-free gradient elution ion-exchange chromatography ICS-2000 (Dionex, USA), the model solutions of oxalate and formate ions, and leachates from soils of the Kola Peninsula. The optimal gradient program was established for separation and detection of oxalate and formate ions in water solutions by ion chromatography. A stability indicating method was developed for the simultaneous determination of water-soluble organic acids in soils. The method has shown high detection limits such as 0.03 mg/L for oxalate ion and 0.02 mg/L for formate ion. High signal reproducibility was achieved in wide range of intensities which correspond to the following ion concentrations: from 0.04 mg/g to 10 mg/L (formate), from 0.1 mg/g to 25 mg/L (oxalate). The concentration of formate and oxalate ions in soil samples is from 0.04 to 0.9 mg/L and 0.45 to 17 mg/L respectively.

  2. Immobilization of soluble protein complexes in MAS solid-state NMR: Sedimentation versus viscosity.

    PubMed

    Sarkar, Riddhiman; Mainz, Andi; Busi, Baptiste; Barbet-Massin, Emeline; Kranz, Maximilian; Hofmann, Thomas; Reif, Bernd

    2016-01-01

    In recent years, MAS solid-state NMR has emerged as a technique for the investigation of soluble protein complexes. It was found that high molecular weight complexes do not need to be crystallized in order to obtain an immobilized sample for solid-state NMR investigations. Sedimentation induced by sample rotation impairs rotational diffusion of proteins and enables efficient dipolar coupling based cross polarization transfers. In addition, viscosity contributes to the immobilization of the molecules in the sample. Natural Deep Eutectic Solvents (NADES) have very high viscosities, and can replace water in living organisms. We observe a considerable amount of cross polarization transfers for NADES solvents, even though their molecular weight is too low to yield significant sedimentation. We discuss how viscosity and sedimentation both affect the quality of the obtained experimental spectra. The FROSTY/sedNMR approach holds the potential to study large protein complexes, which are otherwise not amenable for a structural characterization using NMR. We show that using this method, backbone assignments of the symmetric proteasome activator complex (1.1MDa), and high quality correlation spectra of non-symmetric protein complexes such as the prokaryotic ribosome 50S large subunit binding to trigger factor (1.4MDa) are obtained. PMID:27017576

  3. Laboratory investigation of aluminum solubility and solid-phase properties following alum treatment of lake waters.

    PubMed

    Berkowitz, Jacob; Anderson, Michael A; Graham, Robert C

    2005-10-01

    Water samples from two southern California lakes adversely affected by internal nutrient loading were treated with a 20 mg/L dose of Al3+ in laboratory studies to examine Al solubility and solid-phase speciation over time. Alum [Al2(SO4)3 . 18 H2O] applications to water samples from Big Bear Lake and Lake Elsinore resulted in a rapid initial decrease in pH and alkalinity followed by a gradual recovery in pH over several weeks. Dissolved Al concentrations increased following treatment, reaching a maximum of 2.54 mg/L after 17 days in Lake Elsinore water and 0.91 mg/L after 48 days in Big Bear Lake water; concentrations in both waters then decreased to <0.25 mg/L after 150 days. The solid phase was periodically collected and analyzed using X-ray diffraction (XRD), differential scanning calorimetry-thermogravimetric analysis (DSC-TGA), scanning electron microscopy (SEM), and surface area analyses to investigate the nature of the reaction products and crystallinity development over time. Poorly ordered, X-ray amorphous solid phases transformed over time to relatively well-ordered gibbsite, with strong diffraction peaks at 4.8 and 4.3 A. XRD also indicated the formation of a second (possibly aluminosilicate) crystalline phase after 150 days in Lake Elsinore water. Surface areas also decreased over time as crystals reordered to form gibbsite/microcrystalline gibbsite species. DSC-TGA results suggested that the initially formed amorphous Al(OH)3 underwent transformation to >45% gibbsite. These results were supported by geochemical modeling using Visual MINTEQ, with Al solubility putatively controlled by amorphous Al(OH)3 shortly after treatment and approaching that of microcrystalline gibbsite after about 150 days. These findings indicate that Al(OH)3 formed after alum treatment undergoes significant chemical and mineralogical changes that may alter its effectiveness as a reactive barrier to phosphorus release from lake sediments. PMID:16139325

  4. Field and Laboratory Studies of Reactions between Atmospheric Water Soluble Organic Acids and Inorganic Particles

    SciTech Connect

    Wang, Bingbing; Kelly, Stephen T.; Sellon, Rachel E.; Shilling, John E.; Tivanski, Alexei V.; Moffet, Ryan C.; Gilles, Mary K.; Laskin, Alexander

    2013-06-25

    Atmospheric inorganic particles undergo complex heterogeneous reactions that change their physicochemical properties. Depletion of chloride in sea salt particles was reported in previous field studies and was attributed to the acid displacement of chlorides with inorganic acids, such as nitric and sulfuric acids [1-2]. Recently, we showed that NaCl can react with water soluble organic acids (WSOA) and release gaseous hydrochloric acid (HCl) resulting in formation of organic salts [3]. A similar mechanism is also applicable to mixed WSOA/nitrate particles where multi-phase reactions are driven by the volatility of nitric acid. Furthermore, secondary organic material, which is a complex mixture of carboxylic acids, exhibits the same reactivity towards chlorides and nitrates. Here, we present a systematic study of reactions between atmospheric relevant WSOA, SOM, and inorganic salts including NaCl, NaNO3, and Ca(NO3)2 using complementary micro-spectroscopy analysis.

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

    PubMed

    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. PMID:26468038

  6. Foliar reflective film and water deficit increase anthocyanin to soluble solids ratio during berry ripening in Merlot

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Elevated temperature can decrease the ratio of anthocyanins to soluble solids in red-skinned berries and warming trends in grape production regions have raised concern about color to alcohol balance in wines produced from fruit with altered ratios. In this study, we tested the effectiveness of a fol...

  7. Integrated spectral and image analysis of hyperspectral scattering data for prediction of apple fruit firmness and soluble solids content

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Spectral scattering is useful for assessing the firmness and soluble solids content (SSC) of apples. In previous research, mean reflectance extracted from the hyperspectral scattering profiles was used for this purpose since the method is simple and fast and also gives relatively good predictions. T...

  8. Hydroxylamine hydrochloride-acetic acid-soluble and -insoluble fractions of pelagic sediment: Readsorption revisited

    USGS Publications Warehouse

    Piper, D.Z.; Wandless, G.A.

    1992-01-01

    The extraction of the rare earth elements (REE) from deep-ocean pelagic sediment, using hydroxylamine hydrochloride-acetic acid, leads to the separation of approximately 70% of the bulk REE content into the soluble fraction and 30% into the insoluble fraction. The REE pattern of the soluble fraction, i.e., the content of REE normalized to average shale on an element-by-element basis and plotted against atomic number, resembles the pattern for seawater, whereas the pattern, as well as the absolute concentrations, in the insoluble fraction resembles the North American shale composite. These results preclude significant readsorption of the REE by the insoluble phases during the leaching procedure.

  9. Interaction between Tea Polyphenols and Bile Acid Inhibits Micellar Cholesterol Solubility.

    PubMed

    Ogawa, Kazuki; Hirose, Sayumi; Nagaoka, Satoshi; Yanase, Emiko

    2016-01-13

    The molecular mechanism by which tea polyphenols decrease the micellar solubility of cholesterol is not completely clear. To clarify this mechanism, this study investigated the interaction between tea polyphenols (catechins and oolongtheanins) and cholesterol micelles. A nuclear magnetic resonance (NMR) study was performed on a micellar solution containing taurocholic acid and epigallocatechin gallate (EGCg), and high-performance liquid chromatography (HPLC) analysis was carried out on the precipitate and the supernatant that formed when EGCg was added to a cholesterol-micelle solution. The data indicated a regiospecific interaction of EGCg with taurocholic acid. Therefore, the ability of EGCg to lower the solubility of phosphatidylcholine (PC) and cholesterol in micellar solutions can be attributed to their elimination from the micelles due to interaction between taurocholic acids and EGCg. PMID:26651358

  10. Solubility of methanol in low-temperature aqueous sulfuric acid and implications for atmospheric particle composition

    NASA Technical Reports Server (NTRS)

    Iraci, Laura T.; Essin, Andrew M.; Golden, David M.; Hipskind, R. Stephen (Technical Monitor)

    2001-01-01

    Using traditional Knudsen cell techniques, we find well-behaved Henry's law uptake of methanol in aqueous 45 - 70 wt% H2SO4 solutions at temperatures between 197 and 231 K. Solubility of methanol increases with decreasing temperature and increasing acidity, with an effective Henry's law coefficient ranging from 10(exp 5) - 10(exp 8) M/atm. Equilibrium uptake of methanol into sulfuric acid aerosol particles in the upper troposphere and lower stratosphere will not appreciably alter gas-phase concentrations of methanol. The observed room temperature reaction between methanol and sulfuric acid is too slow to provide a sink for gaseous methanol at the temperatures of the upper troposphere and lower stratosphere. It is also too slow to produce sufficient quantities of soluble reaction products to explain the large amount of unidentified organic material seen in particles of the upper troposphere.

  11. The effect of acid hydrolysis pretreatment on crystallinity and solubility of kenaf cellulose membrane

    SciTech Connect

    Saidi, Anis Syuhada Mohd; Zakaria, Sarani; Chia, Chin Hua; Jaafar, Sharifah Nabihah Syed; Padzil, Farah Nadia Mohammad

    2015-09-25

    Cellulose was extracted from kenaf core pulp (KCP) by series of bleaching steps in the sequence (DEED) where D and E are referred as acid and alkali treatment. The bleached kenaf pulp (BKCP) is then pretreated with acid hydrolysis at room temperature for 1 and 3 h respectively. The pretreated cellulose is dissolved in lithium hydroxide/urea (LiOH/urea) and cellulose solution produced was immersed in distilled water bath. BKCP without treatment was also conducted for comparison purpose. The effects of acid hydrolysis pretreatment on solubility and crystallinity are investigated. Higher solubility of cellulose solution is achieved for treated samples. Cellulose II formation and crystallinity index of the cellulose membrane were determined by X-ray diffraction (XRD)

  12. The effect of acid hydrolysis pretreatment on crystallinity and solubility of kenaf cellulose membrane

    NASA Astrophysics Data System (ADS)

    Saidi, Anis Syuhada Mohd; Zakaria, Sarani; Chia, Chin Hua; Jaafar, Sharifah Nabihah Syed; Padzil, Farah Nadia Mohammad

    2015-09-01

    Cellulose was extracted from kenaf core pulp (KCP) by series of bleaching steps in the sequence (DEED) where D and E are referred as acid and alkali treatment. The bleached kenaf pulp (BKCP) is then pretreated with acid hydrolysis at room temperature for 1 and 3 h respectively. The pretreated cellulose is dissolved in lithium hydroxide/urea (LiOH/urea) and cellulose solution produced was immersed in distilled water bath. BKCP without treatment was also conducted for comparison purpose. The effects of acid hydrolysis pretreatment on solubility and crystallinity are investigated. Higher solubility of cellulose solution is achieved for treated samples. Cellulose II formation and crystallinity index of the cellulose membrane were determined by X-ray diffraction (XRD).

  13. Efficient Route to Highly Water-Soluble Aromatic Cyclic Hydroxamic Acid Ligands

    SciTech Connect

    Seitz, Michael; Raymond, Kenneth N.

    2008-02-06

    2-Hydroxyisoquinolin-1-one (1,2-HOIQO) is a new member of the important class of aromatic cyclic hydroxamic acid ligands which are widely used in metal sequestering applications and metal chelating therapy. The first general approach for the introduction of substituents at the aromatic ring of the chelating moiety is presented. As a useful derivative, the highly water-soluble sulfonic acid has been synthesized by an efficient route that allows general access to 1,2-HOQIO 3-carboxlic acid amides, which are the most relevant for applications.

  14. Interactions in the solid state. II: Interaction of sodium bicarbonate with substituted benzoic acids in the presence of moisture

    SciTech Connect

    Wright, J.L.; Carstensen, J.T.

    1986-06-01

    The interaction of an organic acid with sodium bicarbonate in water produces an effervescent reaction. The reaction products are carbon dioxide, water, and the sodium salt of the acid. The kinetic rate-determining step for this reaction is the dehydration of carbonic acid. The solid-solid interaction with known amounts of moisture was followed by quantitatively determining carbon dioxide evolution as a function of time. The aqueous solubilities, diffusion coefficients, dissociation constants, and solid-solid interaction rates of six different substituted benzoic acids were determined. Using a model based on diffusion of the organic acid through the aqueous layer coupled with chemical reaction, predicted rates and levels of carbon dioxide production were compared with experimental results. Included in the model were the effects of the reaction products on the solution properties of the reactants. It was found that high concentrations of substituted sodium benzoate were generated very quickly and affected the solubility of the reactants, diffusion coefficient of the acid, and the carbonic acid dehydration rate constant. Moisture content was found to have a profound influence on the interaction rate. Water provides a medium for diffusion of the reacting species as well as the reaction solvent.

  15. Acidic Properties and Structure-Activity Correlations of Solid Acid Catalysts Revealed by Solid-State NMR Spectroscopy.

    PubMed

    Zheng, Anmin; Li, Shenhui; Liu, Shang-Bin; Deng, Feng

    2016-04-19

    Solid acid materials with tunable structural and acidic properties are promising heterogeneous catalysts for manipulating and/or emulating the activity and selectivity of industrially important catalytic reactions. On the other hand, the performances of acid-catalyzed reactions are mostly dictated by the acidic features, namely, type (Brønsted vs Lewis acidity), amount, strength, and local environment of acid sites. The latter is relevant to their location (intra- vs extracrystalline), and possible confinement and Brønsted-Lewis acid synergy effects that may strongly affect the host-guest interactions, reaction mechanism, and shape selectivity of the catalytic system. This account aims to highlight some important applications of state-of-the-art solid-state NMR (SSNMR) techniques for exploring the structural and acidic properties of solid acid catalysts as well as their catalytic performances and relevant reaction pathway invoked. In addition, density functional theory (DFT) calculations may be exploited in conjunction with experimental SSNMR studies to verify the structure-activity correlations of the catalytic system at a microscopic scale. We describe in this Account the developments and applications of advanced ex situ and/or in situ SSNMR techniques, such as two-dimensional (2D) double-quantum magic-angle spinning (DQ MAS) homonuclear correlation spectroscopy for structural investigation of solid acids as well as study of their acidic properties. Moreover, the energies and electronic structures of the catalysts and detailed catalytic reaction processes, including the identification of reaction species, elucidation of reaction mechanism, and verification of structure-activity correlations, made available by DFT theoretical calculations were also discussed. Relevant discussions will focus primarily on results obtained from our laboratories in the past decade, including (i) quantitative and qualitative acidity characterization utilizing assorted probe molecules

  16. Solubility of the Sodium and Ammonium Salts of Oxalic Acid in Water with Ammonium Sulfate.

    PubMed

    Buttke, Lukas G; Schueller, Justin R; Pearson, Christian S; Beyer, Keith D

    2016-08-18

    The solubility of the sodium and ammonium salts of oxalic acid in water with ammonium sulfate present has been studied using differential scanning calorimetry, X-ray crystallography, and infrared spectroscopy. The crystals that form from aqueous mixtures of ammonium sulfate/sodium hydrogen oxalate were determined to be sodium hydrogen oxalate monohydrate under low ammonium sulfate conditions and ammonium hydrogen oxalate hemihydrate under high ammonium sulfate conditions. Crystals from aqueous mixtures of ammonium sulfate/sodium oxalate were determined to be ammonium oxalate monohydrate under moderate to high ammonium sulfate concentrations and sodium oxalate under low ammonium sulfate concentrations. It was also found that ammonium sulfate enhances the solubility of the sodium oxalate salts (salting in effect) and decreases the solubility of the ammonium oxalate salts (salting out effect). In addition, a partial phase diagram for the ammonium hydrogen oxalate/water system was determined. PMID:27482644

  17. Solid/liquid phase diagram of the ammonium sulfate/succinic acid/water system.

    PubMed

    Pearson, Christian S; Beyer, Keith D

    2015-05-14

    We have studied the low-temperature phase diagram and water activities of the ammonium sulfate/succinic acid/water system using differential scanning calorimetry and infrared spectroscopy of thin films. Using the results from our experiments, we have mapped the solid/liquid ternary phase diagram, determined the water activities based on the freezing point depression, and determined the ice/succinic acid phase boundary as well as the ternary eutectic composition and temperature. We also compared our results to the predictions of the extended AIM aerosol thermodynamics model (E-AIM) and found good agreement for the ice melting points in the ice primary phase field of this system; however, differences were found with respect to succinic acid solubility temperatures. We also compared the results of this study with those of previous studies that we have published on ammonium sulfate/dicarboxylic acid/water systems. PMID:25431860

  18. Influence of manufacturing factors on physical stability and solubility of solid dispersions containing a low glass transition temperature drug.

    PubMed

    Sakurai, Atsushi; Sako, Kazuhiro; Maitani, Yoshie

    2012-01-01

    In this study, we investigated the effect of manufacturing factors such as particle size, water content and manufacturing method on the physical stability and solubility of solid dispersion formulations of a low-glass-transition-temperature (T(g)) drug. Solid dispersions were prepared from polyvinylpyrrolidone (PVP) and hydroxypropylmethylcellulose (HPMC) by hot melt extrusion or spray drying. Water content of solid dispersions prepared by hot melt extrusion determined by dynamic moisture sorption measurement was increased drastically with relative humidity below a certain level of particle size. The blends with a lower water content (0.8%) prepared by hot melt extrusion during storage were more stable than those with a higher water content (3.5%) prepared by spray drying, which caused rapid recrystallization. Physical stability in the hot melt blends may be attributed to reduced molecular mobility due to a higher T(g). Dissolution study revealed that solid dispersions prepared by hot melt extrusion with the smallest particle size showed decreased solubility, attributed to reduced wetting properties (surface energy), which is not predictable by the Noyes-Whitney equation. Taken together, these results indicate that the control of particle size concerned in water content or wetting properties is critical to ensuring the physical stability or enhancing solubility of low-T(g) drugs. Further, hot melt extrusion, which can reduce water content, is a suitable manufacturing method for solid dispersions of low-T(g) drugs. PMID:23124559

  19. Characterization of a soluble phosphatidic acid phosphatase in bitter melon (Momordica charantia).

    PubMed

    Cao, Heping; Sethumadhavan, Kandan; Grimm, Casey C; Ullah, Abul H J

    2014-01-01

    Momordica charantia is often called bitter melon, bitter gourd or bitter squash because its fruit has a bitter taste. The fruit has been widely used as vegetable and herbal medicine. Alpha-eleostearic acid is the major fatty acid in the seeds, but little is known about its biosynthesis. As an initial step towards understanding the biochemical mechanism of fatty acid accumulation in bitter melon seeds, this study focused on a soluble phosphatidic acid phosphatase (PAP, 3-sn-phosphatidate phosphohydrolase, EC 3.1.3.4) that hydrolyzes the phosphomonoester bond in phosphatidate yielding diacylglycerol and P(i). PAPs are typically categorized into two subfamilies: Mg(2+)-dependent soluble PAP and Mg(2+)-independent membrane-associated PAP. We report here the partial purification and characterization of an Mg(2+)-independent PAP activity from developing cotyledons of bitter melon. PAP protein was partially purified by successive centrifugation and UNOsphere Q and S columns from the soluble extract. PAP activity was optimized at pH 6.5 and 53-60 °C and unaffected by up to 0.3 mM MgCl2. The K(m) and Vmax values for dioleoyl-phosphatidic acid were 595.4 µM and 104.9 ηkat/mg of protein, respectively. PAP activity was inhibited by NaF, Na(3)VO(4), Triton X-100, FeSO4 and CuSO4, but stimulated by MnSO4, ZnSO4 and Co(NO3)2. In-gel activity assay and mass spectrometry showed that PAP activity was copurified with a number of other proteins. This study suggests that PAP protein is probably associated with other proteins in bitter melon seeds and that a new class of PAP exists as a soluble and Mg(2+)-independent enzyme in plants. PMID:25203006

  20. Characterization of a Soluble Phosphatidic Acid Phosphatase in Bitter Melon (Momordica charantia)

    PubMed Central

    Cao, Heping; Sethumadhavan, Kandan; Grimm, Casey C.; Ullah, Abul H. J.

    2014-01-01

    Momordica charantia is often called bitter melon, bitter gourd or bitter squash because its fruit has a bitter taste. The fruit has been widely used as vegetable and herbal medicine. Alpha-eleostearic acid is the major fatty acid in the seeds, but little is known about its biosynthesis. As an initial step towards understanding the biochemical mechanism of fatty acid accumulation in bitter melon seeds, this study focused on a soluble phosphatidic acid phosphatase (PAP, 3-sn-phosphatidate phosphohydrolase, EC 3.1.3.4) that hydrolyzes the phosphomonoester bond in phosphatidate yielding diacylglycerol and Pi. PAPs are typically categorized into two subfamilies: Mg2+-dependent soluble PAP and Mg2+-independent membrane-associated PAP. We report here the partial purification and characterization of an Mg2+-independent PAP activity from developing cotyledons of bitter melon. PAP protein was partially purified by successive centrifugation and UNOsphere Q and S columns from the soluble extract. PAP activity was optimized at pH 6.5 and 53–60°C and unaffected by up to 0.3 mM MgCl2. The Km and Vmax values for dioleoyl-phosphatidic acid were 595.4 µM and 104.9 ηkat/mg of protein, respectively. PAP activity was inhibited by NaF, Na3VO4, Triton X-100, FeSO4 and CuSO4, but stimulated by MnSO4, ZnSO4 and Co(NO3)2. In-gel activity assay and mass spectrometry showed that PAP activity was copurified with a number of other proteins. This study suggests that PAP protein is probably associated with other proteins in bitter melon seeds and that a new class of PAP exists as a soluble and Mg2+-independent enzyme in plants. PMID:25203006

  1. Placement in an acidic environment increase the solubility of white mineral trioxide aggregate

    PubMed Central

    Yavari, Hamid Reza; Borna, Zahra; Rahimi, Saeed; Shahi, Shahriar; Valizadeh, Hadi; Ghojazadeh, Morteza

    2013-01-01

    Aims: The aim of the present study was to evaluate solubility of white mineral trioxide aggregate (WMTA) in an acidic environment. Materials and Methods: Twenty-four metal rings were prepared, filled with WMTA and randomly divided into two groups. The samples in groups 1 and 2 were set in synthetic tissue fluid with pH values of 7.4 and 4.4, respectively and then were transferred to beakers containing synthetic tissue fluid with pH values of 7.7 and 4.4. Solubility of WMTA samples were calculated at the 9 experimental intervals. Data was analyzed with two-factor ANOVA and Bonferroni test (P < 0.03). Results: The total solubility of WMTA in groups 1 and 2 were −9.1796 ± 1.9158% and −1.1192 ± 2.6236%, (P = 0.028) with weight changes of 9.1574 ± 2.1432% and 7.3276 ± 1.5823%, respectively (P = 0.002). Statistical analysis revealed significant differences between the two groups. Conclusions: It was concluded that solubility of WMTA increases in acidic environments and additional therapeutic precautions should be taken to decrease inflammation in endodontic treatment. PMID:23833462

  2. Effect of magnesium carbonate on the solubility, dissolution and oral bioavailability of fenofibric acid powder as an alkalising solubilizer.

    PubMed

    Kim, Kyeong Soo; Kim, Jeong Hyun; Jin, Sung Giu; Kim, Dong Wuk; Kim, Dong Shik; Kim, Jong Oh; Yong, Chul Soon; Cho, Kwan Hyung; Li, Dong Xun; Woo, Jong Soo; Choi, Han-Gon

    2016-04-01

    To investigate the possibility of developing a novel oral pharmaceutical product using fenofibric acid instead of choline fenofibrate, the powder properties, solubility, dissolution and pharmacokinetics in rats of fenofibrate, choline fenofibrate and fenofibric acid were compared. Furthermore, the effect of magnesium carbonate, an alkalising agent on the solubility, dissolution and oral bioavailability of fenofibric acid was assessed, a mixture of fenofibric acid and magnesium carbonate being prepared by simple blending at a weight ratio of 2/1. The three fenofibrate derivatives showed different particle sizes and melting points with similar crystalline shape. Fenofibric acid had a significantly higher aqueous solubility and dissolution than fenofibrate, but significantly lower solubility and dissolution than choline fenofibrate. However, the fenofibric acid/magnesium carbonate mixture greatly improved the solubility and dissolution of fenofibric acid with an enhancement to levels similar with those for choline fenofibrate. Fenofibric acid gave lower plasma concentrations, AUC and Cmax values compared to choline fenofibrate in rats. However, the mixture resulted in plasma concentrations, AUC and Cmax values levels not significantly different from those for choline fenofibrate. Specifically, magnesium carbonate increased the aqueous solubility, dissolution and bioavailability of fenofibric acid by about 7.5-, 4- and 1.6-fold, respectively. Thus, the mixture of fenofibric acid and magnesium carbonate at the weight ratio of 2/1 might be a candidate for an oral pharmaceutical product with improved oral bioavailability. PMID:26992922

  3. Hygroscopic Properties of Internally Mixed Particles Composed of NaCl and Water-Soluble Organic Acids

    SciTech Connect

    Ghorai, Suman; Wang, Bingbing; Tivanski, Alexei V.; Laskin, Alexander

    2014-02-18

    Atmospheric aging of naturally emitted marine aerosol often leads to formation of internally mixed particles composed of sea salts and water soluble organic compounds of anthropogenic origin. Mixing of sea salt and organic components has profound effects on the evolving chemical composition and hygroscopic properties of the resulted particles, which are poorly understood. Here, we have studied chemical composition and hygroscopic properties of laboratory generated NaCl particles mixed with malonic acid (MA) and glutaric acid (GA) at different molar ratios using micro-FTIR spectroscopy and X-ray elemental microanalysis.Hygroscopic properties of inte rnally mixed NaCl and organic acid particles were distinctly different from pure components and varied significantly with the type and amount of organic compound present. Experimental results were in a good agreement with the AIM modeling calculations of gas/liquid/solid partitioning in studied systems. X-ray elemental microanalysis of particles showed that Cl/Na ratio decreased with increasing organic acid component in the particles with MA yielding lower ratios relative to GA. We attribute the depletion of chloride to the formation of Na-malonate and Na-glutarate salts resulted by HCl evaporation from dehydrating particles.

  4. Hygroscopic properties of internally mixed particles composed of NaCl and water-soluble organic acids.

    PubMed

    Ghorai, Suman; Wang, Bingbing; Tivanski, Alexei; Laskin, Alexander

    2014-02-18

    Atmospheric aging of naturally emitted marine aerosol often leads to formation of internally mixed particles composed of sea salts and water-soluble organic compounds of anthropogenic origin. Mixing of sea salt and organic components has profound effects on the evolving chemical composition and hygroscopic properties of the resulted particles, which are poorly understood. Here, we have studied chemical composition and hygroscopic properties of laboratory generated NaCl particles mixed with malonic acid (MA) and glutaric acid (GA) at different molar ratios using micro-FTIR spectroscopy, atomic force microscopy, and X-ray elemental microanalysis. Hygroscopic properties of internally mixed NaCl and organic acid particles were distinctly different from pure components and varied significantly with the type and amount of organic compound present. Experimental results were in a good agreement with the AIM modeling calculations of gas/liquid/solid partitioning in studied systems. X-ray elemental microanalysis of particles showed that Cl/Na ratio decreased with increasing organic acid component in the particles with MA yielding lower ratios relative to GA. We attribute the depletion of chloride to the formation of sodium malonate and sodium glutarate salts resulted by HCl evaporation from dehydrating particles. PMID:24437520

  5. [Prediction the Soluble Solid Content in Sugarcanes by Using Near Infrared Hyperspectral Imaging System].

    PubMed

    Gao, Jun-feng; Zhang, Chu; Xie, Chuan-qi; Zhu, Feng-le; Guo, Zhen-hao; He, Yong

    2015-08-01

    In order to explore the feasibility of prediction soluble solid contents (SSC) in sugarcane stalks by using near infrared hyperspectral imaging techniques, two hundred and forty sugarcane stalks which come from three different varieties were studied. After obtaining the raw hyperspectral images of sugarcane stalks, the spectral information and textural features were discussed respectively. The prediction models were established by using partial least squares regression (PLSR), principal components regression (PCR) and least squares support vector machines (LS-SVM) algorithms. Besides, three different selected wavelengths algorithms such as successive projection (SPA) algorithms, intervals partial least squares (iPLS) algorithms and uninformation variables elimination (UVE) algorithm were analyzed after building partial least squares regression model. The results indicate that partial least squares regression model based on spectral features can be an steady model to predict SSC and the correlation coefficient (R2) of calibration sets and prediction sets are 0.879, 0.843. The root mean square errors of calibration sets and prediction sets are 0.644, 0.742 respectively. The obtained 105 wavelengths which were selected by UVE algorithm are effective spectral features. The R2 results of calibration sets and prediction sets of its PLSR model are 0.860, 0.813. The root mean square errors of calibration sets and prediction sets are 0.693, 0.810 respectively PMID:26672284

  6. Nondestructive evaluation of soluble solid content in strawberry by near infrared spectroscopy

    NASA Astrophysics Data System (ADS)

    Guo, Zhiming; Huang, Wenqian; Chen, Liping; Wang, Xiu; Peng, Yankun

    This paper indicates the feasibility to use near infrared (NIR) spectroscopy combined with synergy interval partial least squares (siPLS) algorithms as a rapid nondestructive method to estimate the soluble solid content (SSC) in strawberry. Spectral preprocessing methods were optimized selected by cross-validation in the model calibration. Partial least squares (PLS) algorithm was conducted on the calibration of regression model. The performance of the final model was back-evaluated according to root mean square error of calibration (RMSEC) and correlation coefficient (R2 c) in calibration set, and tested by mean square error of prediction (RMSEP) and correlation coefficient (R2 p) in prediction set. The optimal siPLS model was obtained with after first derivation spectra preprocessing. The measurement results of best model were achieved as follow: RMSEC = 0.2259, R2 c = 0.9590 in the calibration set; and RMSEP = 0.2892, R2 p = 0.9390 in the prediction set. This work demonstrated that NIR spectroscopy and siPLS with efficient spectral preprocessing is a useful tool for nondestructively evaluation SSC in strawberry.

  7. Neural network and principal component regression in non-destructive soluble solids content assessment: a comparison.

    PubMed

    Chia, Kim-seng; Abdul Rahim, Herlina; Abdul Rahim, Ruzairi

    2012-02-01

    Visible and near infrared spectroscopy is a non-destructive, green, and rapid technology that can be utilized to estimate the components of interest without conditioning it, as compared with classical analytical methods. The objective of this paper is to compare the performance of artificial neural network (ANN) (a nonlinear model) and principal component regression (PCR) (a linear model) based on visible and shortwave near infrared (VIS-SWNIR) (400-1000 nm) spectra in the non-destructive soluble solids content measurement of an apple. First, we used multiplicative scattering correction to pre-process the spectral data. Second, PCR was applied to estimate the optimal number of input variables. Third, the input variables with an optimal amount were used as the inputs of both multiple linear regression and ANN models. The initial weights and the number of hidden neurons were adjusted to optimize the performance of ANN. Findings suggest that the predictive performance of ANN with two hidden neurons outperforms that of PCR. PMID:22302428

  8. Neural network and principal component regression in non-destructive soluble solids content assessment: a comparison*

    PubMed Central

    Chia, Kim-seng; Abdul Rahim, Herlina; Abdul Rahim, Ruzairi

    2012-01-01

    Visible and near infrared spectroscopy is a non-destructive, green, and rapid technology that can be utilized to estimate the components of interest without conditioning it, as compared with classical analytical methods. The objective of this paper is to compare the performance of artificial neural network (ANN) (a nonlinear model) and principal component regression (PCR) (a linear model) based on visible and shortwave near infrared (VIS-SWNIR) (400–1000 nm) spectra in the non-destructive soluble solids content measurement of an apple. First, we used multiplicative scattering correction to pre-process the spectral data. Second, PCR was applied to estimate the optimal number of input variables. Third, the input variables with an optimal amount were used as the inputs of both multiple linear regression and ANN models. The initial weights and the number of hidden neurons were adjusted to optimize the performance of ANN. Findings suggest that the predictive performance of ANN with two hidden neurons outperforms that of PCR. PMID:22302428

  9. Rapid assessment of soluble solids content in navel orange by near-infrared diffuse reflectance spectra

    NASA Astrophysics Data System (ADS)

    Liu, Yande; Luo, Ji; Chen, Xingmiao; Ying, Yibin

    2006-10-01

    The potential of using Near Infrared diffuse reflectance spectroscopy to assess soluble solids content (SSC) of intact navel orange was examined. A total 40 samples were used to develop the calibration and prediction models. NIR spectral data were collected in the spectral region between 350 nm and 2500 nm and its second derivative spectra was used for this study. Different scattering correction algorithms (no preprocessing and multiplicative scattering correction (MSC) were compared. Calibration models based on different spectral ranges, different derivatives and different kinds of statistical models including partial least square (PLS) and principle component regression (PCR) were also compared in this research. The best results of PLS models with the second derivative spectra are r=0.929, RMSEC=0.517 and RMSEP=0.592, in the wavelength range of 361-2488 nm. The segment length used to derivate the spectra influences the calibration model and the results are better when the segment lengths and gap sizes are lower in Norris derivate filter. The results show that this method is feasible for rapid assessing SSC of the navel orange.

  10. Regulation of Bile Acid Synthesis by Fat-soluble Vitamins A and D*

    PubMed Central

    Schmidt, Daniel R.; Holmstrom, Sam R.; Fon Tacer, Klementina; Bookout, Angie L.; Kliewer, Steven A.; Mangelsdorf, David J.

    2010-01-01

    Bile acids are required for proper absorption of dietary lipids, including fat-soluble vitamins. Here, we show that the dietary vitamins A and D inhibit bile acid synthesis by repressing hepatic expression of the rate-limiting enzyme CYP7A1. Receptors for vitamin A and D induced expression of Fgf15, an intestine-derived hormone that acts on liver to inhibit Cyp7a1. These effects were mediated through distinct cis-acting response elements in the promoter and intron of Fgf15. Interestingly, transactivation of both response elements appears to be required to maintain basal Fgf15 expression levels in vivo. Furthermore, whereas induction of Fgf15 by vitamin D is mediated through its receptor, the induction of Fgf15 by vitamin A is mediated through the retinoid X receptor/farnesoid X receptor heterodimer and is independent of bile acids, suggesting that this heterodimer functions as a distinct dietary vitamin A sensor. Notably, vitamin A treatment reversed the effects of the bile acid sequestrant cholestyramine on Fgf15, Shp, and Cyp7a1 expression, suggesting a potential therapeutic benefit of vitamin A under conditions of bile acid malabsorption. These results reveal an unexpected link between the intake of fat-soluble vitamins A and D and bile acid metabolism, which may have evolved as a means for these dietary vitamins to regulate their own absorption. PMID:20233723

  11. Organic acids as cloud condensation nuclei: Laboratory studies of highly soluble and insoluble species

    NASA Astrophysics Data System (ADS)

    Pradeep Kumar, P.; Broekhuizen, K.; Abbatt, J. P. D.

    2003-05-01

    The ability of sub-micron-sized organic acid particles to act as cloud condensation nuclei (CCN) has been examined at room temperature using a newly constructed continuous-flow, thermal-gradient diffusion chamber (TGDC). The organic acids studied were: oxalic, malonic, glutaric, oleic and stearic. The CCN properties of the highly soluble acids - oxalic, malonic and glutaric - match very closely Köhler theory predictions which assume full dissolution of the dry particle and a surface tension of the growing droplet equal to that of water. In particular, for supersaturations between 0.3 and 0.6, agreement between the dry particle diameter which gives 50% activation and that calculated from Köhler theory is to within 3nm on average. In the course of the experiments, considerable instability of glutaric acid particles was observed as a function of time and there is evidence that they fragment to some degree to smaller particles. Stearic acid and oleic acid, which are both highly insoluble in water, did not activate at supersaturations of 0.6% with dry diameters up to 140nm. Finally, to validate the performance of the TGDC, we present results for the activation of ammonium sulfate particles that demonstrate good agreement with Köhler theory if solution non-ideality is considered. Our findings support earlier studies in the literature that showed highly soluble organics to be CCN active but insoluble species to be largely inactive.

  12. Sialic Acid Is Required for Neuronal Inhibition by Soluble MAG but not for Membrane Bound MAG.

    PubMed

    Al-Bashir, Najat; Mellado, Wilfredo; Filbin, Marie T

    2016-01-01

    Myelin-Associated Glycoprotein (MAG), a major inhibitor of axonal growth, is a member of the immunoglobulin (Ig) super-family. Importantly, MAG (also known as Siglec-4) is a member of the Siglec family of proteins (sialic acid-binding, immunoglobulin-like lectins), MAG binds to complex gangliosides, specifically GD1a and/or GT1b. Therefore, it has been proposed as neuronal receptors for MAG inhibitory effect of axonal growth. Previously, we showed that MAG binds sialic acid through domain 1 at Arg118 and is able to inhibit axonal growth through domain 5. We developed a neurite outgrowth (NOG) assay, in which both wild type MAG and mutated MAG (MAG Arg118) are expressed on cells. In addition we also developed a soluble form NOG in which we utilized soluble MAG-Fc and mutated MAG (Arg118-Fc). Only MAG-Fc is able to inhibit NOG, but not mutated MAG (Arg118)-Fc that has been mutated at its sialic acid binding site. However, both forms of membrane bound MAG- and MAG (Arg118)- expressing cells still inhibit NOG. Here, we review various results from different groups regarding MAG's inhibition of axonal growth. Also, we propose a model in which the sialic acid binding is not necessary for the inhibition induced by the membrane form of MAG, but it is necessary for the soluble form of MAG. This finding highlights the importance of understanding the different mechanisms by which MAG inhibits NOG in both the soluble fragmented form and the membrane-bound form in myelin debris following CNS damage. PMID:27065798

  13. Sialic Acid Is Required for Neuronal Inhibition by Soluble MAG but not for Membrane Bound MAG

    PubMed Central

    Al-Bashir, Najat; Mellado, Wilfredo; Filbin, Marie T.

    2016-01-01

    Myelin-Associated Glycoprotein (MAG), a major inhibitor of axonal growth, is a member of the immunoglobulin (Ig) super-family. Importantly, MAG (also known as Siglec-4) is a member of the Siglec family of proteins (sialic acid-binding, immunoglobulin-like lectins), MAG binds to complex gangliosides, specifically GD1a and/or GT1b. Therefore, it has been proposed as neuronal receptors for MAG inhibitory effect of axonal growth. Previously, we showed that MAG binds sialic acid through domain 1 at Arg118 and is able to inhibit axonal growth through domain 5. We developed a neurite outgrowth (NOG) assay, in which both wild type MAG and mutated MAG (MAG Arg118) are expressed on cells. In addition we also developed a soluble form NOG in which we utilized soluble MAG-Fc and mutated MAG (Arg118-Fc). Only MAG-Fc is able to inhibit NOG, but not mutated MAG (Arg118)-Fc that has been mutated at its sialic acid binding site. However, both forms of membrane bound MAG- and MAG (Arg118)- expressing cells still inhibit NOG. Here, we review various results from different groups regarding MAG’s inhibition of axonal growth. Also, we propose a model in which the sialic acid binding is not necessary for the inhibition induced by the membrane form of MAG, but it is necessary for the soluble form of MAG. This finding highlights the importance of understanding the different mechanisms by which MAG inhibits NOG in both the soluble fragmented form and the membrane-bound form in myelin debris following CNS damage. PMID:27065798

  14. Solid Phase Synthesis of C-Terminal Boronic Acid Peptides.

    PubMed

    Behnam, Mira A M; Sundermann, Tom R; Klein, Christian D

    2016-05-01

    Peptides and peptidomimetics with a C-terminal boronic acid group have prolific applications in numerous fields of research, but their synthetic accessibility remains problematic. A convenient, high yield synthesis of peptide-boronic acids on a solid support is described here, using commercially available 1-glycerol polystyrene resin. The method is compatible with Fmoc chemistry and offers a versatile approach to aryl and alkyl aminoboronic acids without additional purification steps. PMID:27104613

  15. Design, optimization and evaluation of glipizide solid self-nanoemulsifying drug delivery for enhanced solubility and dissolution.

    PubMed

    Dash, Rajendra Narayan; Mohammed, Habibuddin; Humaira, Touseef; Ramesh, Devi

    2015-10-01

    A solid self-nanoemulsifying drug-delivery system (solid SNEDDS) has been explored to improve the solubility and dissolution profile of glipizide. SNEDDS preconcentrate was systematically optimized using a circumscribed central composite design by varying Captex 355 (Oil), Solutol HS15 (Surfactant) and Imwitor 988 (Co-surfactant). The optimized SNEDDS preconcentrate consisted of Captex 355 (30% w/w), Solutol HS15 (45% w/w) and Imwitor 988 (25% w/w). The saturation solubility (SS) of glipizide in optimized SNEDDS preconcentrate was found to be 45.12 ± 1.36 mg/ml, indicating an improvement (1367 times) of glipizide solubility as compared to its aqueous solubility (0.033 ± 0.0021 mg/ml). At 90% SS, glipizide was loaded to the optimized SNEDDS. In-vitro dilution of liquid SNEDDS resulted in a nanoemulsion with a mean droplet size of 29.4 nm. TEM studies of diluted liquid SNEDDS confirmed the uniform shape and size of the globules. The liquid SNEDDS was adsorbed onto calcium carbonate and talc to form solid SNEDDS. PXRD, DSC, and SEM results indicated that, the presence of glipizide as an amorphous and as a molecular dispersion state within solid SNEDDS. Glipizide dissolution improved significantly (p < 0.001) from the solid SNEDDS (∼100% in 15 min) as compared to the pure drug (18.37%) and commercial product (65.82) respectively. PMID:26594119

  16. Design, optimization and evaluation of glipizide solid self-nanoemulsifying drug delivery for enhanced solubility and dissolution

    PubMed Central

    Dash, Rajendra Narayan; Mohammed, Habibuddin; Humaira, Touseef; Ramesh, Devi

    2015-01-01

    A solid self-nanoemulsifying drug-delivery system (solid SNEDDS) has been explored to improve the solubility and dissolution profile of glipizide. SNEDDS preconcentrate was systematically optimized using a circumscribed central composite design by varying Captex 355 (Oil), Solutol HS15 (Surfactant) and Imwitor 988 (Co-surfactant). The optimized SNEDDS preconcentrate consisted of Captex 355 (30% w/w), Solutol HS15 (45% w/w) and Imwitor 988 (25% w/w). The saturation solubility (SS) of glipizide in optimized SNEDDS preconcentrate was found to be 45.12 ± 1.36 mg/ml, indicating an improvement (1367 times) of glipizide solubility as compared to its aqueous solubility (0.033 ± 0.0021 mg/ml). At 90% SS, glipizide was loaded to the optimized SNEDDS. In-vitro dilution of liquid SNEDDS resulted in a nanoemulsion with a mean droplet size of 29.4 nm. TEM studies of diluted liquid SNEDDS confirmed the uniform shape and size of the globules. The liquid SNEDDS was adsorbed onto calcium carbonate and talc to form solid SNEDDS. PXRD, DSC, and SEM results indicated that, the presence of glipizide as an amorphous and as a molecular dispersion state within solid SNEDDS. Glipizide dissolution improved significantly (p < 0.001) from the solid SNEDDS (∼100% in 15 min) as compared to the pure drug (18.37%) and commercial product (65.82) respectively. PMID:26594119

  17. The Interplay between Inorganic Phosphate and Amino Acids determines Zinc Solubility in Brain Slices

    PubMed Central

    Rumschik, Sean M.; Nydegger, Irma; Zhao, Jinfu; Kay, Alan R

    2009-01-01

    Inorganic phosphate (Pi) is an important polyanion needed for ATP synthesis and bone formation. Since it is found at millimolar levels in plasma it is usually incorporated as a constituent of artificial cerebrospinal fluid (ACSF) formulations for maintaining brain slices. In this paper we show that Pi limits the extracellular zinc concentration by inducing metal precipitation. We present data suggesting that amino acids like histidine may counteract the Pi-induced zinc precipitation by the formation of soluble zinc complexes. We propose that the interplay between Pi and amino acids in the extracellular space may influence the availability of metals for cellular uptake. PMID:19183267

  18. Modified mass action law-based model to correlate the solubility of solids and liquids in entrained supercritical carbon dioxide.

    PubMed

    González, J C; Vieytes, M R; Botana, A M; Vieites, J M; Botana, L M

    2001-02-23

    The solubility of solids and liquids in supercritical CO2 with added entrainers was modeled with a modified version of the equation of Chrastil to include the effect of entrainers. By considering the formation of the solute-entrainer-solvent complexes an equation is obtained which predicts an exponential increase of solubility with fluid density and/or entrainer concentration. The correlating model was tested by non-linear regression through a computerized iterative process for several systems where an entrainer was present. Four experimental parameters are easily regressed from experimental data, hence the corresponding properties of components such as chemical potentials or critical parameters are not needed. Instead of its simplicity, this thermodynamical model provided a good correlation of the solubility enhancement in the presence of entrainer effect. PMID:11263564

  19. Reactions Between Water Soluble Organic Acids and Nitrates in Atmospheric Aerosols: Recycling of Nitric Acid and Formation of Organic Salts

    SciTech Connect

    Wang, Bingbing; Laskin, Alexander

    2014-03-25

    Atmospheric particles often include a complex mixture of nitrate and secondary organic materials accumulated within the same individual particles. Nitrate as an important inorganic component can be chemically formed in the atmosphere. For instance, formation of sodium nitrate (NaNO3) and calcium nitrate Ca(NO3)2 when nitrogen oxide and nitric acid (HNO3) species react with sea salt and calcite, respectively. Organic acids contribute a significant fraction of photochemically formed secondary organics that can condense on the preexisting nitrate-containing particles. Here, we present a systematic microanalysis study on chemical composition of laboratory generated particles composed of water soluble organic acids and nitrates (i.e. NaNO3 and Ca(NO3)2) investigated using computer controlled scanning electron microscopy with energy dispersive analysis of X-rays (CCSEM/EDX) and Fourier transform infrared micro-spectroscopy (micro-FTIR). The results show that water-soluble organic acids can react with nitrates releasing gaseous HNO3 during dehydration process. These reactions are attributed to acid displacement of nitrate with weak organic acids driven by the evaporation of HNO3 into gas phase due to its relatively high volatility. The reactions result in significant nitrate depletion and formation of organic salts in mixed organic acids/nitrate particles that in turn may affect their physical and chemical properties relevant to atmospheric environment and climate. Airborne nitrate concentrations are estimated by thermodynamic calculations corresponding to various nitrate depletions in selected organic acids of atmospheric relevance. The results indicate a potential mechanism of HNO3 recycling, which may further affect concentrations of gas- and aerosol-phase species in the atmosphere and the heterogeneous reaction chemistry between them.

  20. On-line detection of orange soluble solid content using visible and near infrared transmission measurements

    NASA Astrophysics Data System (ADS)

    Fu, Xiaping; Ying, Yibin; Xu, Huirong; Qi, Bing; Xie, Lijuan

    2012-05-01

    A prototype of on-line system developed by ourselves was used to non-destructively inspect orange quality. This system includes three main parts: machine vision part for fruit external quality detection, visible and near infrared (Vis-NIR) spectroscopy part for fruit internal quality detection, and weighing part for fruit weight detection. Fruit scrolled on the roller in the machine vision part, while stopped scrolling before entering the Vis-NIR spectroscopy part. Therefore, fruit positions and directions were inconsistent for spectra acquisition. This paper was aimed to study the influence of fruit detection orientation on spectra variation and model estimation performance using the on-line system. The system was configured to operate at typical grader speeds (0.27m/s or approximately three fruit per second) and detect the light transmitted through oranges. Stepwise multi linear regression models were developed for fruit with consistent directions and inconsistent directions in the wavelength range of 600-950 nm, and gave reasonable calibration correlations R2=0.89-0.92 and low cross validation errors (RMSECV=0.44-0.56%). The calibration model with spherical samples only turned out the best prediction results, which has lowest RMSEP of 0.56%-0.63% for different fruit orientations. It can be seen from the study that fruit shape would influence the fruit orientation for spectra aqcuiring of spherical samples after scrolling, and would further influence the modeling resutls. It is better to acquire spectra and establish models for sampels with different shapes separately and then applying them based on shape detection resutls to improve the soluble solid content (SSC) prediction accuracy.

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

    PubMed Central

    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 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 °Brix (QL); 0.58 °Brix (ZC)], low RMSEC [0.48 °Brix (QL); 0.34 °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 nondestructive way. PMID:17266185

  2. Molecular interaction studies of amorphous solid dispersions of the antimelanoma agent betulinic acid.

    PubMed

    Yu, Meiki; Ocando, Joseph E; Trombetta, Louis; Chatterjee, Parnali

    2015-04-01

    Betulinic acid (BA), a novel natural product with antimelanoma activity, has poor aqueous solubility (<0.1 μg/mL) and therefore exhibits poor bioavailability. The purpose of this study was to explore the feasibility of preparing BA solid dispersions (BA-SDs) with hydrophilic polymers to enhance the aqueous solubility of BA. Melt-quenched solid dispersions (MQ-SDs) of BA were prepared at various ratios with the hydrophilic polymers including Soluplus, HPMCAS-HF, Kollidon VA64, Kollidon K90, and Eudragit RLPO. BA was found to be miscible in all polymers at a 1:4 (w/w) ratio by modulated differential scanning calorimetry (MDSC). BA/Soluplus MQ-SD exhibited the highest solubility in simulated body fluids followed by BA/Kollidon VA64 MQ-SD. The MQ-SDs of BA/Soluplus, BA/HPMCAS-HF, and BA/Kollidon VA64 were found to be amorphous as indicated by X-ray powder diffraction (XRPD) studies. Fourier transform infra-red (FT-IR) studies indicated molecular interactions between BA and Soluplus. Our preliminary screening of polymers indicates that Soluplus and Kollidon VA64 exhibit the greatest potential to form BA-SDs. PMID:25331193

  3. Bioreduction of uranium(VI) complexed with citric acid by Clostridia affects its structure and solubility.

    PubMed

    Francis, A J; Dodge, C J

    2008-11-15

    Uranium contamination of the environment from mining and milling operations, nuclear-waste disposal, and ammunition use is a widespread global problem. Natural attenuation processes such as bacterial reductive precipitation and immobilization of soluble uranium is gaining much attention. However, the presence of naturally occurring organic ligands can affect the precipitation of uranium. Here, we report that the anaerobic spore-forming bacteria Clostridia, ubiquitous in soils, sediments, and wastes, capable of reduction of Fe(III) to Fe(II), Mn(IV) to Mn(II), U(VI) to U(IV), Pu(IV) to Pu(III), and Tc(VI) to Tc(IV); reduced U(VI) associated with citric acid in a dinuclear 2:2 U(VI): citric acid complex to a biligand mononuclear 1:2 U(IV):citric acid complex,which remained in solution, in contrast to reduction and precipitation of uranium. Our findings show that U(VI) complexed with citric acid is readily accessible as an electron acceptor despite the inability of the bacterium to metabolize the complexed organic ligand. Furthermore, it suggests that the presence of organic ligands at uranium-contaminated sites can affect the mobility of the actinide under both oxic and anoxic conditions by forming such soluble complexes. PMID:19068806

  4. Chemical constituents: water-soluble vitamins, free amino acids and sugar profile from Ganoderma adspersum.

    PubMed

    Kıvrak, İbrahim

    2015-01-01

    Ganoderma adspersum presents a rigid fruiting body owing to chitin content and having a small quantity of water or moisture. The utility of bioactive constituent of the mushroom can only be available by extraction for human usage. In this study, carbohydrate, water-soluble vitamin compositions and amino acid contents were determined in G. adspersum mushroom. The composition in individual sugars was determined by HPLC-RID, mannitol (13.04 g/100 g) and trehalose (10.27 g/100 g) being the most abundant sugars. The examination of water-soluble vitamins and free amino acid composition was determined by UPLC-ESI-MS/MS. Essential amino acid constituted 67.79% of total amino acid, which is well worth the attention with regard to researchers and consumers. In addition, G. adspersum, which is also significantly rich in B group vitamins and vitamin C, can provide a wide range of notable applications in the pharmaceutics, cosmetics, food and dietary supplement industries. G. adspersum revealed its value for pharmacy and nutrition fields. PMID:25169839

  5. Adaption of kinetics to solid electrolyte interphase layer formation and application to electrolyte-soluble reaction products

    NASA Astrophysics Data System (ADS)

    Gourdin, Gerald; Zheng, Dong; Qu, Deyang

    2015-12-01

    During the electrochemical lithiation of a carbon electrode, carbonate-based electrolytes react with the electrode surface and undergo reductive decomposition to form a solid electrolyte interphase (SEI) layer that passivates the surface of the carbon electrode. In addition, reduction of the electrolyte also results in the generation of electrolyte-soluble products. Structural similarities between the soluble and insoluble products provide an opportunity to examine the formation kinetics of the SEI layer through an analysis of the kinetic behavior of the soluble products. In this work, the electrolyte-soluble products generated by reductive decomposition of a baseline electrolyte were analyzed at different stages and at different hold times during the initial lithiation of an amorphous carbon electrode. A statistical regression analysis of that data was used to produce a representative lithiation experiment from which was calculated the potential-dependent formation rates for the soluble decomposition products. The predicted formation rate data was fitted using an adapted rate equation that accounts for the effect of the SEI layer to obtain estimated formation rate constants and redox potentials.

  6. Solid Acid Fuel Cell Stack for APU Applications

    SciTech Connect

    Duong, Hau H.

    2011-04-15

    Solid acid fuel cell technology affords the opportunity to operate at the 200-300 degree centigrade regime that would allow for more fuel flexibility, compared to polymer electrode membrane fuel cell, while avoiding the relatively more expensive and complex system components required by solid oxide fuel cell. This project addresses many factors such as MEA size scalability, fuel robustness, stability, etc., that are essential for successful commercialization of the technology.

  7. Isotope composition of carbon in amino acids of solid bitumens

    NASA Astrophysics Data System (ADS)

    Shanina, S. N.; Bushnev, D. A.

    2014-06-01

    Primary data are presented on the isotope composition of carbon in individual amino acids from solid bitumens and several biological objects. The amino acids of biological objects are characterized by wide variations of the isotope composition of carbon. This fact occurs owing to the difference in biochemical paths of metabolism resulting in the synthesis of individual amino acids. The δ13C values are somewhat decreased for individual amino acids in asphaltenes, varying from -7.7 to -31.7‰. The carbon of amino acids is weighted in kerits from Bad'el' compared to asphaltenes. All the natural bitumens retain the characteristic trend for natural substances: the isotopically heavy and light amino acids by carbon are glycine and leucine, respectively. The isotope composition of amino-acid carbon is lightened compared to natural bitumens in the samples formed under a pronounced thermal impact (asphalt-like crust and kirishite).

  8. Development and characterization of solid dispersion-microsphere controlled release system for poorly water-soluble drug.

    PubMed

    Malipeddi, Venkata Ramana; Dua, Kamal; Awasthi, Rajendra

    2016-10-01

    The present study aimed to improve solubility and prolong the release duration of a poorly soluble drug using a combination of two different types of formulations (solid dispersion and microspheres). The solid dispersions were prepared by fusion method using urea and mannitol as hydrophilic carriers. Microspheres were prepared by solvent evaporation method using Eudragit L-100 (EL100) and Eudragit RS PO (ERS) as rate-controlling polymers. Flurbiprofen (FBP)-urea (1:2) solid dispersion and microspheres of FBP-EL-100-ERS (1:0.25:0.75) were used for the development of controlled release formulation by mixing them in different proportions. The FBP-containing formulations were evaluated for percentage yield, drug content, morphology, in vitro release, and in vivo anti-inflammatory activity. The best selected formulation was further evaluated for the controlled and improved effects. SEM photomicrograph confirmed the spherical shape of microspheres and with particle size in the range of 73.5-85.4 μm. In vitro release of FBP from controlled release formulations indicated that the formulation containing solid dispersion:microspheres (1:0.5) yielded prolonged effect up to 10 h. The release kinetics followed zero-order, and the mechanism of drug release was found to be diffusion rate controlled. This formulation had shown better inhibition of edema of rat paw up to 16 h and identified as a suitable product for controlled delivery of FBP. In conclusion, the concept of using a binary mixture of solid dispersion and microspheres can be used for other drugs that exhibit a poor solubility in stomach pH and a faster release in intestinal pH. PMID:27343081

  9. Lysophosphatidic acids are new substrates for the phosphatase domain of soluble epoxide hydrolase[S

    PubMed Central

    Oguro, Ami; Imaoka, Susumu

    2012-01-01

    Soluble epoxide hydrolase (sEH) is a bifunctional enzyme that has a C-terminus epoxide hydrolase domain and an N-terminus phosphatase domain. The endogenous substrates of epoxide hydrolase are known to be epoxyeicosatrienoic acids, but the endogenous substrates of the phosphatase activity are not well understood. In this study, to explore the substrates of sEH, we investigated the inhibition of the phosphatase activity of sEH toward 4-methylumbelliferyl phosphate by using lecithin and its hydrolyzed products. Although lecithin itself did not inhibit the phosphatase activity, the hydrolyzed lecithin significantly inhibited it, suggesting that lysophospholipid or fatty acid can inhibit it. Next, we investigated the inhibition of phosphatase activity by lysophosphatidyl choline, palmitoyl lysophosphatidic acid, monopalmitoyl glycerol, and palmitic acid. Palmitoyl lysophosphatidic acid and fatty acid efficiently inhibited phosphatase activity, suggesting that lysophosphatidic acids (LPAs) are substrates for the phosphatase activity of sEH. As expected, palmitoyl, stearoyl, oleoyl, and arachidonoyl LPAs were efficiently dephosphorylated by sEH (Km, 3–7 μM; Vmax, 150–193 nmol/min/mg). These results suggest that LPAs are substrates of sEH, which may regulate physiological functions of cells via their metabolism. PMID:22217705

  10. [Huanghua pear soluble solids contents Vis/NIR spectroscopy by analysis of variables optimization and FICA].

    PubMed

    Xu, Wen-li; Sun, Tong; Hu, Tian; Hu, Tao; Liu, Mu-hua

    2014-12-01

    The purpose of this study was to establish a mathematical model of the visible/near-infrared (Vis/NIR) diffuse transmission spectroscopy with fine stability and precise predictability for the non destructive testing of the soluble solids content of huanghua pear, through comparing the effects of various pretreatment methods, variable optimization method, fast independent principal component analysis (FICA) and least squares support vector machines (LS-SVM) on mathematica model for SSC of huanghua pear, and the best combination of methods to establish model for SSC of huanghua pear was got. Vis/NIR diffuse transmission spectra of huanghua pear were acquired by a Quality Spec spectrometer, three methods including genetic algorithm, successive projections algorithm and competitive adaptive reweighted sampling (CARS) were used firstly to select characteristic variables from spectral data of huanghua pears in the wavelength range of 550~950 nm, and then FICA was used to extract factors from the characteristic variables, finally, validation model for SSC in huanghua pears was built by LS-SVM on the basic of those parameters got above. The results showed that using LS-SVM on the foundation of the 21 variables screened by CARS and the 12 factors selected by FICA, the CARS-FICA-LS-SVM regression model for SSC in huanghua pears was built and performed best, the coefficient of determination and root mean square error of calibration and prediction sets were RC(2)=0.974, RMSEC=0.116%, RP(2)=0.918, and RMSEP=0.158% respectively, and compared with the mathematical model which uses PLS as modeling method, the number of variables was down from 401 to 21, the factors were also down from 14 to 12, the coefficient of determination of modeling and prediction sets were up to 0.023 and 0.019 respectively, while the root mean square errors of calibration and prediction sets were reduced by 0.042% and 0.010% respectively. These experimental results showed that using CARS-FICA-LS-SVM to

  11. Solubility and Reaction Rates of Aluminum Solid Phases Under Geothermal Conditions

    SciTech Connect

    Benezeth, P.; Palmer, D.A.; Wesolowski, D.J.; Anovitz, L.M.

    2000-05-28

    Experimental studies involving equilibrium solubility and dissolution/precipitation rates were initiated on aluminum hydroxide phases prevalent under geothermal reservoir conditions. A large capacity, hydrogen-electrode concentration cell (HECC) was constructed specifically for this purpose.

  12. Soluble species in the Arctic summer troposphere - Acidic gases, aerosols, and precipitation

    NASA Technical Reports Server (NTRS)

    Talbot, R. W.; Vijgen, A. S.; Harriss, R. C.

    1992-01-01

    The large-scale spatial distribution from 0.15-to 6 km altitude in the North American Arctic troposphere of several soluble acidic gases and major aerosol species during the summertime is reported. The distribution is found to be compositionally consistent on a large spatial scale. The summertime troposphere is an acidic environment, with HCOOH and CH3COOH the principal acidic gases while acidic sulfate aerosols dominate the particulate phase. There appears to be a surface source of NH3 over the pack ice which may originate from decay of dead marine organisms on the ice surface, evolution from surface ocean waters in open ice leads, or release from rotting sea ice. At low altitude over the pack ice this NH34 appears to partially neutralize aerosol acidity. Over sub-Arctic tundra in southeastern Alaska, inputs of marine biogenic sulfur from the Bering Sea appear to be an important source of boundary layer aerosol SO4(2-). The rainwater acidity over the tundra is typical of remote regions.

  13. Phosphorylated Mesoporous Carbon as a Solid Acid Catalyst

    SciTech Connect

    Dai, Sheng; Mayes, Richard T; Fulvio, Pasquale F; Ma, Zhen

    2011-01-01

    Mesoporous carbon catalyst supports are attractive due to their wide chemical stability while potentially increasing masstransport through and providing a path for larger molecules to access catalytic sites. Herein we report the synthesis of a 10 phosphorylated mesoporous carbon solid-acid catalyst characterized by NH3-TPD and isopropanol dehydration.

  14. Chlorin p6-Based Water-Soluble Amino Acid Derivatives as Potent Photosensitizers for Photodynamic Therapy.

    PubMed

    Meng, Zhi; Yu, Bin; Han, Guiyan; Liu, Minghui; Shan, Bin; Dong, Guoqiang; Miao, Zhenyuan; Jia, Ningyang; Tan, Zou; Li, Buhong; Zhang, Wannian; Zhu, Haiying; Sheng, Chunquan; Yao, Jianzhong

    2016-05-26

    The development of novel photosensitizer with high phototoxicity, low dark toxicity, and good water solubility is a challenging task for photodynamic therapy (PDT). A series of chlorin p6-based water-soluble amino acid conjugates were synthesized and investigated for antitumor activity. Among them, aspartylchlorin p6 dimethylester (7b) showed highest phototoxicity against melanoma cells with weakest dark toxicity, which was more phototoxic than verteporfin while with less dark toxicity. It also exhibited better in vivo PDT antitumor efficacy on mice bearing B16-F10 tumor than verteporfin. The biological assays revealed that 7b was localized in multiple subcellular organelles and could cause both cell necrosis and apoptosis after PDT in a dose-dependent manner, resulting in more effective cell destruction. As a result, 7b represents a promising photosensitizer for PDT applications because of its strong absorption in the phototherapeutic window, relatively high singlet oxygen quantum yield, highest dark toxicity/phototoxicity ratio, good water solubility, and excellent in vivo PDT antitumor efficacy. PMID:27136389

  15. Preparation of Carboxymethylchitosan Nanoparticles with Acid-Sensitive Bond Based on Solid Dispersion of 10-Hydroxycamptothecin

    PubMed Central

    Yao, Risheng; Liu, Lu; Deng, Shengsong; Ren, Weitao

    2011-01-01

    Solid dispersions were prepared by a conventional solvent evaporation method from the water-insoluble model drug 10-hydroxycamptothecin (HCPT) and monomethoxypoly(ethylene glycol) 2000 (mPEG 2000). And then one type of novel biodegradable nanoparticles, the solid dispersion (HCPT/mPEG-CHO) grafted with carboxymethylchitosan (HCPT/mPEG-g-CMCTS) was synthesized. The increase in HCPT solubility of solid dispersion was up to 21-fold compared with the original drug. With the increasing of the amount of mPEG-CHO, solubility of HCPT was from 7.71 μg/mL to 25.82 μg/mL. Colloid systems based on solid dispersion were stable in aqueous medium at 5°C. After 5 months storage at 25°C, the solid dispersions do not change at all. HCPT/mPEG-g-CMCTS was synthesized by grafting reaction of carboxymethylchitosan with mPEG-CHO to form Schiff base which is sensitive to acid environment. The release rate of HCPT from this conjugate in pH 5.4 was much higher than that in the environment of pH 7.4 and p H 4.5. The cumulative release percentages are 45%, 25%, and 15%, respectively. The cumulative release percentage of HCPT in conjugate was only 15% within 85 h while the original drug was up to 70% in pH 7.4, showing a significant slow-release property. This drug model can be attractive candidates as delivery biosystems in tumor therapy. PMID:22389854

  16. Influence of neutral salts on the hydrothermal stability of acid-soluble collagen.

    PubMed

    Brown, E M; Farrell, H M; Wildermuth, R J

    2000-02-01

    The thermal stability of acid-soluble collagens was studied by circular dichroism (CD) spectroscopy. Adult bovine dermal collagen (BDC), rat-tail tendon collagen (RTC), and calf skin collagen (CSC) were compared. Despite some variability in amino acid composition and apparent molecular weight, the CD spectra for helical and unordered collagen structures were essentially the same for all the sources. The melting of these collagens occurs as a two-stage process characterized by a pretransition (Tp) followed by complete denaturation (Td). The characteristic temperatures vary with the source of the collagen; for mature collagens (BDC, RTC) Tp = 30 degrees C and Td = 36 degrees C, and for CSC Tp = 34 degrees C and Td = 40 degrees C. Neutral salts, NaCl or KCl, at low concentrations (0.02-0.2 M) appear to bind to the collagens and shift the thermal transitions of these collagens to lower temperatures. PMID:10945432

  17. Effects of excess pantothenic acid administration on the other water-soluble vitamin metabolisms in rats.

    PubMed

    Shibata, Katsumi; Takahashi, Chisato; Fukuwatari, Tsutomu; Sasaki, Ryuzo

    2005-12-01

    To acquire the data concerning the tolerable upper intake level which prevents health problems from an excessive intake of pantothenic acid, an animal experiment was done. Rats of the Wistar strain (male, 3 wk old) were fed on a diet which contains 0%, 0.0016% (control group), 1%, or 3% calcium pantothenate for 29 d. The amount of weight increase, the food intake, and the organ weights were measured, as well as the pantothenic acid contents in urine, the liver and blood. Moreover, to learn the influence of excessive pantothenic acid on other water-soluble vitamin metabolism, thiamin, riboflavin, a vitamin B6 catabolite, the niacin catabolites, and ascorbic acid in urine were measured. As for the 3% addition group, enlargement of the testis, diarrhea, and hair damage were observed, and the amount of weight increase and the food intake were less than those of the control group. However, abnormality was not seen in the 1% addition group. The amount of pantothenic acid in urine, the liver, and blood showed a high correlation with intake level of pantothenic acid. It was only for 4-pyridoxic acid, a vitamin B6 catabolite, in urine that a remarkable difference was observed against the control group. Moreover, the (2-Py+4-Py)/MNA excretion ratio for these metabolites of the nicotinamide also indicated a low value in the 3% pantothenic acid group. As for the calcium pantothenate, it was found that the 3% level in the diet was the lowest-observed-adverse-effect-level (LOAEL) and the 1% level was the no-observed-adverse-effect-level (NOAEL). PMID:16521696

  18. The Solubility of Xenon in Simple Organic Solvents and in Aqueous Amino Acid Solutions.

    NASA Astrophysics Data System (ADS)

    Himm, Jeffrey Frank

    We have measured the Ostwald solubility (L) of ('133)Xe in a variety of liquids, including normal alkanes, normal alkanols, and aqueous solutions of amino acids, NaCl, and sucrose. For the alkanes and alkanols, measurements were made in the temperature range from 10-50(DEGREES)C. Values of L were found to decrease with increasing temperature, and also with increasing chain length, for both series of solvents. Thermodynamic properties of solution (enthalpy and entropy of solution) are calculated using both mole fraction and number density scales. Results are interpreted using Uhlig's model of the solvation process. Measurements of L in aqueous amino acid solutions were made at 25(DEGREES)C. Concentrations of amino acids in solution varied from near saturation for each of the amino acids studied to pure water. In all solutions, except those with NaCl, L decreases linearly with increasing solution molarity. Hydration numbers (H), the mean number of water molecules associated with each solute molecule, were determined for each amino acid, for NaCl, and for sucrose. Values of H obtained ranged from near zero (arginine, H = 0.2 (+OR-) 0.5) to about 16 (NaCl, H = 16.25 (+OR-) 0.3).

  19. Kinetics during the redox biotransformation of pollutants mediated by immobilized and soluble humic acids.

    PubMed

    Cervantes, Francisco J; Martínez, Claudia M; Gonzalez-Estrella, Jorge; Márquez, Arturo; Arriaga, Sonia

    2013-03-01

    The aim of this study was to elucidate the kinetic constraints during the redox biotransformation of the azo dye, Reactive Red 2 (RR2), and carbon tetrachloride (CT) mediated by soluble humic acids (HAs) and immobilized humic acids (HAi), as well as by the quinoid model compounds, anthraquinone-2,6-disulfonate (AQDS) and 1,2-naphthoquinone-4-sulfonate (NQS). The microbial reduction of both HAs and HAi by anaerobic granular sludge (AGS) was the rate-limiting step during decolorization of RR2 since the reduction of RR2 by reduced HAi proceeded at more than three orders of magnitute faster than the electron-transferring rate observed during the microbial reduction of HAi by AGS. Similarly, the reduction of RR2 by reduced AQDS proceeded 1.6- and 1.9-fold faster than the microbial reduction of AQDS by AGS when this redox mediator (RM) was supplied in soluble and immobilized form, respectively. In contrast, the reduction of NQS by AGS occurred 1.6- and 19.2-fold faster than the chemical reduction of RR2 by reduced NQS when this RM was supplied in soluble and immobilized form, respectively. The microbial reduction of HAs and HAi by a humus-reducing consortium proceeded 1,400- and 790-fold faster than the transfer of electrons from reduced HAs and HAi, respectively, to achieve the reductive dechlorination of CT to chloroform. Overall, the present study provides elucidation on the rate-limiting steps involved in the redox biotransformation of priority pollutants mediated by both HAs and HAi and offers technical suggestions to overcome the kinetic restrictions identified in the redox reactions evaluated. PMID:22565330

  20. Soluble adenylyl cyclase is an acid-base sensor in epithelial base-secreting cells.

    PubMed

    Roa, Jinae N; Tresguerres, Martin

    2016-08-01

    Blood acid-base regulation by specialized epithelia, such as gills and kidney, requires the ability to sense blood acid-base status. Here, we developed primary cultures of ray (Urolophus halleri) gill cells to study mechanisms for acid-base sensing without the interference of whole animal hormonal regulation. Ray gills have abundant base-secreting cells, identified by their noticeable expression of vacuolar-type H(+)-ATPase (VHA), and also express the evolutionarily conserved acid-base sensor soluble adenylyl cyclase (sAC). Exposure of cultured cells to extracellular alkalosis (pH 8.0, 40 mM HCO3 (-)) triggered VHA translocation to the cell membrane, similar to previous reports in live animals experiencing blood alkalosis. VHA translocation was dependent on sAC, as it was blocked by the sAC-specific inhibitor KH7. Ray gill base-secreting cells also express transmembrane adenylyl cyclases (tmACs); however, tmAC inhibition by 2',5'-dideoxyadenosine did not prevent alkalosis-dependent VHA translocation, and tmAC activation by forskolin reduced the abundance of VHA at the cell membrane. This study demonstrates that sAC is a necessary and sufficient sensor of extracellular alkalosis in ray gill base-secreting cells. In addition, this study indicates that different sources of cAMP differentially modulate cell biology. PMID:27335168

  1. PULMONARY INJURY AND INFLAMMATION FROM REPEATED EXPOSURE TO SOLUBLE COMPONENTS AND SOLID PARTICULATE MATTER (PM)

    EPA Science Inventory

    Pulmonary injury from acute exposures to PM and the role of soluble versus insoluble PM have received considerable attention; however, their long-term impacts are less well understood. This study compared pulmonary injury and inflammatory responses from repeated exposure to solub...

  2. CARDIAC INJURY FROM LONG TERM EPISODIC EXPOSURE TO PARTICULATE MATTER (PM): SOLUBLE COMPONENTS OR SOLID PARTICLES?

    EPA Science Inventory

    Long-term exposure to PM has been associated with cardiac injury in rats. The purpose of this study was to investigate if cardiac injury was due to soluble metals (i.e., zinc), insoluble PM, or pulmonary injury/inflammation. Male Wistar Kyoto rats (n=8) were exposed intratracheal...

  3. Interlaboratory evaluation of cellulosic acid-soluble internal air sampling capsules for multi-element analysis.

    PubMed

    Andrews, Ronnee N; Feng, H Amy; Ashley, Kevin

    2016-01-01

    An interlaboratory study was carried out to evaluate the use of acid-soluble cellulosic air sampling capsules for their suitability in the measurement of trace elements in workplace atmospheric samples. These capsules are used as inserts to perform closed-face cassette sample collection for occupational exposure monitoring. The interlaboratory study was performed in accordance with NIOSH guidelines that describe statistical procedures for evaluating measurement accuracy of air monitoring methods. The performance evaluation materials used consisted of cellulose acetate capsules melded to mixed-cellulose ester filters that were dosed with multiple elements from commercial standard aqueous solutions. The cellulosic capsules were spiked with the following 33 elements of interest in workplace air monitoring: Ag, Al, As, Ba, Be, Ca, Cd, Co, Cr, Cu, Fe, In, K, La, Li, Mg, Mn, Mo, Ni, P, Pb, Sb, Se, Sn, Sr, Te, Ti, Tl, V, W, Y, Zn, Zr. The elemental loading levels were certified by an accredited provider of certified reference materials. Triplicates of media blanks and multielement-spiked capsules at three different elemental loadings were sent to each participating laboratory; the elemental loading levels were not revealed to the laboratories. The volunteer participating laboratories were asked to prepare the samples by acid dissolution and to analyze aliquots of extracted samples by inductively coupled plasma atomic emission spectrometry in accordance with NIOSH methods. It was requested that the study participants report their analytical results in units of μg of each target element per internal capsule sample. For the majority of the elements investigated (30 out of 33), the study accuracy estimates obtained satisfied the NIOSH accuracy criterion (A < 25%). This investigation demonstrates the utility of acid-soluble internal sampling capsules for multielement analysis by atomic spectrometry. PMID:26308974

  4. Solid phase sequencing of double-stranded nucleic acids

    DOEpatents

    Fu, Dong-Jing; Cantor, Charles R.; Koster, Hubert; Smith, Cassandra L.

    2002-01-01

    This invention relates to methods for detecting and sequencing of target double-stranded nucleic acid sequences, to nucleic acid probes and arrays of probes useful in these methods, and to kits and systems which contain these probes. Useful methods involve hybridizing the nucleic acids or nucleic acids which represent complementary or homologous sequences of the target to an array of nucleic acid probes. These probe comprise a single-stranded portion, an optional double-stranded portion and a variable sequence within the single-stranded portion. The molecular weights of the hybridized nucleic acids of the set can be determined by mass spectroscopy, and the sequence of the target determined from the molecular weights of the fragments. Nucleic acids whose sequences can be determined include nucleic acids in biological samples such as patient biopsies and environmental samples. Probes may be fixed to a solid support such as a hybridization chip to facilitate automated determination of molecular weights and identification of the target sequence.

  5. Conversion of biomass into 5-hydroxymethylfurfural using solid acid catalyst.

    PubMed

    Yang, Fengli; Liu, Qishun; Bai, Xuefang; Du, Yuguang

    2011-02-01

    5-Hydroxymethylfurfural (HMF) was produced from monosaccharide (fructose and glucose), polysaccharide (inulin) and the Jerusalem artichoke juice by a simple one-pot reaction including hydrolysis and dehydration using solid acid under mild condition. Hydrated niobium pentoxide (Nb(2)O(5)·nH(2)O(2)) after pretreatment showed high catalytic activities for dehydration of mono- and polysaccharide to HMF at 433 K in water-2-butanol (2:3 v/v) biphasic system, giving high HMF yield of 89% and 54% from fructose and inulin, respectively. The HMF yield was up to 74% and 65% when inulin and Jerusalem artichoke juice were hydrolyzed by exoinulinase. The solid acid made the process environment-friendly and energy-efficient to convert carbohydrates into bio-fuels and platform chemicals. PMID:21036606

  6. Profiling of soluble neutral oligosaccharides from treated biomass using solid phase extraction and LC-TOF MS.

    PubMed

    Vismeh, Ramin; Humpula, James F; Chundawat, Shishir P S; Balan, Venkatesh; Dale, Bruce E; Jones, A Daniel

    2013-05-15

    Thermochemical pretreatments of cellulosic biomass are known to improve cell wall enzymatic digestibility, while simultaneously releasing substantial amounts of soluble oligosaccharides. Profiling of oligosaccharides released during pretreatment yields information essential for choosing glycosyl hydrolases necessary for cost-effective conversion of cellulosic biomass to desired biofuel/biochemical end-products. In this report we present a methodology for profiling of soluble neutral oligosaccharides released from ammonia fiber expansion (AFEX™)-pretreated corn stover. Our methodology employs solid phase extraction (SPE) enrichment of oligosaccharides using porous graphitized carbon (PGC), followed by high performance liquid chromatography (HPLC) separation using a polymeric amine based column and electrospray ionization time-of-flight mass spectrometry (ESI-TOF-MS). For structural elucidation on the chromatographic time scale, nonselective multiplexed collision-induced dissociation was performed for quasi-simultaneous acquisition of oligosaccharide molecular and fragment masses in a single analysis. These analyses revealed glucans up to degree of polymerization (DP) 22 without modifications. Additionally, arabinoxylans up to DP=6 were detected in pretreated biomass extracts (post-enzymatic digestion). Cross-ring fragment ion abundances were consistent with assignment of linkages between sugar units in glucans and also xylose backbone in arabinoxylans as 1-4 linkages. Comprehensive profiling of soluble oligosaccharides also demonstrated decreases in levels of acetate esters of arabinoxylan oligosaccharides with concomitant increases in nonacetylated oligosaccharides that were consistent with earlier observations of 85% release of acetate esters by AFEX™ pretreatment. PMID:23544634

  7. Isolation and characterization of acid-soluble collagen from the scales of marine fishes from Japan and Vietnam.

    PubMed

    Minh Thuy, Le Thi; Okazaki, Emiko; Osako, Kazufumi

    2014-04-15

    Acid-soluble collagen (ASC) was successfully extracted from the scales of lizard fish (Saurida spp.) and horse mackerel (Trachurus japonicus) from Japan and Vietnam and grey mullet (Mugil cephalis), flying fish (Cypselurus melanurus) and yellowback seabream (Dentex tumifrons) from Japan. ASC yields were about 0.43-1.5% (on a dry weight basis), depending on the species. The SDS-PAGE profile showed that the ASCs were type I collagens, and consisted of two different α chains, α1 and α2, as well as a β component. ASC of horse mackerel from Vietnam contained a higher imino acid level than that from Japan. ASC denaturation temperature (Td) ranged from 26 to 29 °C, depending on fish species and imino acid content (p<0.01). Maximal solubility of individual collagens was observed at pHs 1-3. Collagen solubility decreased sharply at NaCl concentrations >0.4M, regardless of fish type. PMID:24295705

  8. Electrospun nanofibers as a potential controlled-release solid dispersion system for poorly water-soluble drugs.

    PubMed

    Paaver, Urve; Heinämäki, Jyrki; Laidmäe, Ivo; Lust, Andres; Kozlova, Jekaterina; Sillaste, Elen; Kirsimäe, Kalle; Veski, Peep; Kogermann, Karin

    2015-02-01

    Electrospinning was introduced as a novel technique for preparing controlled-release (CR) amorphous solid dispersions (SD) and polymeric nanofibers of a poorly water-soluble drug. Piroxicam (PRX) was used as a low-dose poorly-soluble drug and hydroxypropyl methylcellulose (HPMC) as an amorphous-state stabilising carrier polymer in nanofibers. Raman spectroscopy, X-ray powder diffraction (XPRD), differential scanning calorimetry (DSC) and scanning electron microscopy (SEM) were used in the physical characterisation of the CR-SD nanofibers. Special attention was paid on the effects of a polymer and solvent system on the solid-state properties and physical stability of nanofibers. The average dry diameter of the electrospun CR-SD nanofibers ranged from 400 to 600 nm (SEM). PRX existed in amorphous form in the nanofibers immediately after fabrication and after a short-term (3-month) aging at low temperature (6-8 °C/0% RH) and ambient room temperature (22 °C/0% RH). At higher temperature and humidity (30 °C/85% RH), however, amorphous PRX in the nanofibers tended to slowly recrystallise to PRX form III. The electrospun CR-SD nanofibers exhibited a short lag-time, the absence of initial burst release and zero-order linear CR dissolution kinetics. In conclusion, electrospinning can be used to fabricate supersaturating CR-SD nanofibers of PRX and HPMC, and to stabilise the amorphous state of PRX. PMID:25549852

  9. Artemether-Soluplus Hot-Melt Extrudate Solid Dispersion Systems for Solubility and Dissolution Rate Enhancement with Amorphous State Characteristics

    PubMed Central

    Fule, Ritesh A.; Meer, Tarique S.; Sav, Ajay R.; Amin, Purnima D.

    2013-01-01

    This work studied artemether (ARTM) solid dispersion (SD) formulation using mixture of polymer excipient Soluplus, PEG 400, Lutrol F127, and Lutrol F68 melts at temperatures lower than the melting point of ARTM using a laboratory-size, single-screw rotating batch extruder. The effects of three surfactants PEG 400, Lutrol F127, and Lutrol F68 and parameters like mixing temperature, screw rotating speed, and residence time were systematically studied. SEM, XRD, and FT-IR were employed to investigate the evolution of ARTM's dissolution into the molten excipient. Differential scanning calorimetry (DSC) was used to quantitatively study the melting enthalpy evolution of the drug. The results showed that the dissolution rate increased with increasing the ratio of polymer and surfactant to that of drug. It was concluded that the dissolution of the drug in the polymer melt is a convective diffusion process and that laminar distributive mixing can significantly enhance the dissolution rate. The aqueous solubility and dissolution rate of prepared solid dispersion were significantly enhanced. In vitro antimalarial studies revealed marked improvement in IC50 values. Thus hot-melt extrusion (HME) is a promising technology for improving solubility and dissolution profile of ARTM. PMID:26555968

  10. Pharmacokinetics of salicylic acid following administration of aspirin tablets and three different forms of soluble aspirin in normal subjects.

    PubMed

    Gatti, G; Barzaghi, N; Attardo Parrinello, G; Vitiello, B; Perucca, E

    1989-01-01

    The pharmacokinetic profile of an innovative formulation of soluble aspirin (l-ornithine acetylsalicylate, ldB 1003) was compared with that of conventional tablets and two other soluble dosage forms (d, l-lysine acetylsalicylate and a buffered effervescent formulation of acetylsalicylic acid) after administration of single oral doses in six normal volunteers. All soluble forms showed a rapid absorption profile, peak plasma salicylic acid levels being attained after about 30 min on average and without statistically significant differences among the solutions tested. As compared to the soluble formulations, acetylsalicylic acid given as tablets resulted in slower absorption, with peak plasma salicylic acid levels being reached more than 1 h after dosing. Despite these differences in time course of plasma level profiles, the extent of absorption was similar for all formulations. Apart from the potential advantages in terms of improved gastric tolerability, the increased rate of absorption of aspirin solutions is therapeutically useful whenever a rapid onset of action is required. In this respect, the kinetic pattern of the innovative formulation compares favourably with that of other available soluble dosage forms. PMID:2517497

  11. Solid-state characterization and solubility of a genistein-caffeine cocrystal

    NASA Astrophysics Data System (ADS)

    Sowa, Michał; Ślepokura, Katarzyna; Matczak-Jon, Ewa

    2014-11-01

    Combination of genistein and caffeine leads to a 1:1 cocrystalline phase, which was identified by means of a solvent-drop grinding experiment and isolated afterwards in a solution-evaporation approach. Obtained cocrystal was characterized by X-ray single-crystal and powder diffraction as well as investigated in terms of thermal stability and Hirshfeld surfaces. A scale-up procedure was provided by slurry technique, enabling solubility determination. Neutral forms of both compounds cocrystallize in a common P21/c space group of the monoclinic crystal system. Analysis of packing and interactions in the crystal lattice reveals formation of molecular layers, formed by O-H⋯O, O-H⋯N and C-H⋯O-type contacts between genistein and caffeine molecules, whereas stabilization of the three-dimensional crystal lattice is provided by π⋯π interactions. Dissolution studies in a 50:50 v/v ethanol-water medium revealed that the maximum solubility of the cocrystalline phase reached 0.861 mg/mL after 8 h, revealing some degree of enhancement as compared to parent genistein, maximum solubility of which was also reached after 8 h and equalled 0.588 mg/mL.

  12. Purification and characterization of the acid soluble 26-kDa polypeptide from soybean seeds.

    PubMed

    Momma, M; Haraguchi, K; Saito, M; Chikuni, K; Harada, K

    1997-08-01

    Whey proteins from soybean seeds of Japanese varieties were analyzed by SDS-polyacrylamide gel electrophoresis (SDS-PAGE). Among 11 varieties of soybean, three green and one black soybeans lacked a 26-kDa band that was found in all yellow soybeans. In this paper, the 26-kDa protein was named AS26k (acid soluble 26-kDa protein) temporarily. The AS26k protein was purified from Glycine max cv. Nattosyoryu, which is yellow soybean, through four purification steps: 30-35% saturated ammonium sulfate fractionation, ion exchange chromatography on S Sepharose Fast Flow, gel filtration on Sephadex G-100, and hydrophobic chromatography on phenyl Sepharose CL-4B. Purified AS26k was cleaved with V8 proteinase from Staphylococcus aureus or CNBr. The cleaved polypeptide contained two typical dehydrin motif sequences: DEYGNPV and (M)DKIKEKLPG, and a 19 amino acids sequence similar to a pea dehydrin. Native AS26k had a molecular mass of 32 kDa on gel filtration and a pl of 7.2 on two-dimensional PAGE. Similarly to other dehydrins and late embryogenesis abundant (LEA) proteins, AS26k was rich in hydrophilic amino acids, and highly heat stable. These results showed that AS26k was a dehydrin, a group II LEA protein in soybean seeds. PMID:9301109

  13. The entry of HCl through soluble surfactants on sulfuric acid: effects of chain branching.

    PubMed

    Burden, Daniel K; Johnson, Alexis M; Krier, James M; Nathanson, Gilbert M

    2014-07-17

    Gas-liquid scattering experiments are used to determine how a soluble, branched surfactant (2-ethylbutanol) controls the entry of gaseous HCl molecules into 60 and 68 wt % D2SO4 at 213 K. Short-chain alcohols spontaneously segregate to the surfaces of these sulfuric acid solutions, which are representative of aerosol droplets in the lower stratosphere. We find that 2-ethylbutanol enhances HCl entry at low surface coverages, most likely because it provides extra interfacial OH groups that aid HCl dissociation. This enhancement disappears at higher coverages as the alkyl chains crowd each other and block access to the acid. The branched alcohol impedes HCl entry more effectively than its unbranched isomer 1-hexanol, implying that the larger 2-ethybutanol footprint on the surface blocks more HCl molecules from reaching the alcohol-acid interface. This behavior contrasts sharply with gas transport through long-chain monolayers, where branching introduces gaps that allow more facile passage. The experiments suggest that short-chain surfactants with extended footprints may impede transport more effectively than their unbranched isomers. PMID:24620717

  14. Development and characterisation of sustained release solid dispersion oral tablets containing the poorly water soluble drug disulfiram.

    PubMed

    Shergill, Mandip; Patel, Mina; Khan, Siraj; Bashir, Ayesha; McConville, Christopher

    2016-01-30

    Administration of drugs via the oral route is the most common and preferred route due to its ease of administration, cost-effectiveness and flexibility in design. However, if the drug being administered has limited aqueous solubility it can result in poor bioavailability. Furthermore, the low pH of the stomach as well as enzymatic activity can result in drugs delivered via the oral route being rapidly metabolised and degraded. Here we demonstrate the development and characterisation of sustained release solid dispersion oral tablets, containing the poorly water-soluble drug disulfiram (DSF). The tablets, which are manufactured from two different polymers (Kolliphor(®) P 188 and P 237) specifically designed for the manufacture of solid dispersions and two different polymers (Kollidon(®) SR and HPMC) specifically designed to provide sustained release, can enhance the solubility of DSF, sustain its release, while protecting it from degradation in simulated gastric fluid (SGF). The paper demonstrates that when using the hot melt method at 80°C the DSF loading capacity of the Kolliphor(®) P 188 and P 237 polymers is approximately 43 and 46% respectively, with the DSF completely in an amorphous state. The addition of 80% Kollidon(®) SR to the formulation completely protected the DSF in SGF for up to 70 min with 16% degradation after 120 min, while 75% degradation occurred after 120 min with the addition of 80% HPMC. The release rate of DSF can be manipulated by both the loading and type of sustained release polymer used, with HPMC providing for a much faster release rate compared to Kollidon(®) SR. PMID:26608620

  15. Acid-Soluble Nucleotides in an Asporogenous Mutant of Bacillus subtilis

    PubMed Central

    Chow, C. T.; Takahashi, I.

    1972-01-01

    An asporogenous mutant of Bacillus subtilis Sp−H12-3, which is considered to have a block at stage 0, showed general growth characteristics similar to those of sporulating cultures. However, a sudden increase in the total amount of acid-soluble nucleotides observed at t2 in sporulating bacteria was completely absent in this mutant. In sporulating cells, a marked increase in two nucleotides which were identified to be uridine diphosphate (UDP)-galactose and UDP-N-acetylglucosamine was noted, whereas UDP-glucose appeared to be accumulated in the mutant cells at t2. No unusual nucleotides were found in the strains of B. subtilis examined. The possible role of these UDP derivatives in early stages of sporulation in B. subtilis is discussed. PMID:4622128

  16. Membranotropic properties of the water soluble amino acid and peptide derivatives of fullerene C60.

    PubMed

    Kotelnikova, R A; Kotelnikov, A I; Bogdanov, G N; Romanova, V S; Kuleshova, E F; Parnes, Z N; Vol'pin, M E

    1996-07-01

    The modifying effects of the products of the equimolar addition Of DL-alanine and DL-alanyl-DL-alanine to fullerene C60 on the structure and permeability of the lipid bilayer of phosphatidylcholine liposomes has been studied using the luminescence probe technique. It is shown that these water soluble amino acid and dipeptide derivatives of fullerene (C60-AD) are quenchers of pyrene fluorescence and erythrosine phosphorescence of in both a water solution and liposomes. To study the permeability of the lipid bilayer a procedure based on the triplet probe technique has been developed. It has been found that the C60-AD derivatives under study are able to localize inside the artificial membrane, to penetrate into the liposomes through the lipid bilayer and to perform activated transmembrane transport of bivalent metal ions. PMID:8766810

  17. Conjugated linoleic acid increases in milk from cows fed condensed corn distillers solubles and fish oil.

    PubMed

    Bharathan, M; Schingoethe, D J; Hippen, A R; Kalscheur, K F; Gibson, M L; Karges, K

    2008-07-01

    Twelve lactating Holstein cows were randomly assigned to 1 of 4 experimental diets in a replicated 4 x 4 Latin square design with 4-wk periods to ascertain the lactational response to feeding fish oil (FO), condensed corn distillers solubles (CDS) as a source of extra linoleic acid, or both. Diets contained either no FO or 0.5% FO and either no CDS or 10% CDS in a 2 x 2 factorial arrangement of treatments. Diets were fed as total mixed rations for ad libitum consumption. The forage to concentrate ratio was 55:45 on a dry matter basis for all diets and the diets contained 16.2% crude protein. The ether extract concentrations were 2.86, 3.22, 4.77, and 5.02% for control, FO, CDS, and FOCDS diets, respectively. Inclusion of FO or CDS or both had no effect on dry matter intake, feed efficiency, body weight, and body condition scores compared with diets without FO and CDS, respectively. Yields of milk (33.3 kg/d), energy-corrected milk, protein, lactose, and milk urea N were similar for all diets. Feeding FO and CDS decreased milk fat percentages (3.85, 3.39, 3.33, and 3.12%) and yields compared with diets without FO and CDS. Proportions of trans-11 C18:1 (vaccenic acid), cis-9 trans-11 conjugated linoleic acid (CLA; 0.52, 0.90, 1.11, and 1.52 g/100 g of fatty acids), and trans-10 cis-12 CLA (0.07, 0.14, 0.13, and 0.16 g/100 g of fatty acids) in milk fat were increased by FO and CDS. No interactions were observed between FO and CDS on cis-9 trans-11 CLA although vaccenic acid tended to be higher with the interaction. The addition of CDS to diets increased trans-10 C18:1. Greater ratios of vaccenic acid to cis-9 trans-11 CLA in plasma than in milk fat indicate tissue synthesis of cis-9 trans-11 CLA in the mammary gland from vaccenic acid in cows fed FO or CDS. Feeding fish oil at 0.5% of diet dry matter with a C18:2 n-6 rich source such as CDS increased the milk CLA content but decreased milk fat percentages. PMID:18565937

  18. A win-win solution in oral delivery of lipophilic drugs: supersaturation via amorphous solid dispersions increases apparent solubility without sacrifice of intestinal membrane permeability.

    PubMed

    Miller, Jonathan M; Beig, Avital; Carr, Robert A; Spence, Julie K; Dahan, Arik

    2012-07-01

    Recently, we have revealed a trade-off between solubility increase and permeability decrease when solubility-enabling oral formulations are employed. We have shown this trade-off phenomenon to be ubiquitous, and to exist whenever the aqueous solubility is increased via solubilizing excipients, regardless if the mechanism involves decreased free fraction (cyclodextrins complexation, surfactant micellization) or simple cosolvent solubilization. Discovering a way to increase drug solubility without concomitant decreased permeability represents a major advancement in oral delivery of lipophilic drugs and is the goal of this work. For this purpose, we sought to elucidate the solubility-permeability interplay when increased apparent solubility is obtained via supersaturation from an amorphous solid dispersion (ASD) formulation. A spray-dried ASD of the lipophilic drug progesterone was prepared in the hydrophilic polymer hydroxypropyl methylcellulose acetate succinate (HPMC-AS), which enabled supersaturation up to 4× the crystalline drug's aqueous solubility (8 μg/mL). The apparent permeability of progesterone from the ASD in HPMC-AS was then measured as a function of increasing apparent solubility (supersaturation) in the PAMPA and rat intestinal perfusion models. In contrast to previous cases in which apparent solubility increases via cyclodextrins, surfactants, and cosolvents resulted in decreased apparent permeability, supersaturation via ASD resulted in no decrease in apparent permeability with increasing apparent solubility. As a result, overall flux increased markedly with increasing apparent solubility via ASD as compared to the other formulation approaches. This work demonstrates that supersaturation via ASDs has a subtle yet powerful advantage over other solubility-enabling formulation approaches. That is, increased apparent solubility may be achieved without the expense of apparent intestinal membrane permeability. Thus, supersaturation via ASDs presents a

  19. Solid Lipid Nanoparticles Loaded with Retinoic Acid and Lauric Acid as an Alternative for Topical Treatment of Acne Vulgaris.

    PubMed

    Silva, Elton Luiz; Carneiro, Guilherme; De Araújo, Lidiane Advíncula; Trindade, Mariana de Jesus Vaz; Yoshida, Maria Irene; Oréfice, Rodrigo Lambert; Farias, Luis de Macêdo; De Carvalho, Maria Auxiliadora Roque; Dos Santos, Simone Gonçalves; Goulart, Gisele Assis Castro; Alves, Ricardo José; Ferreira, Lucas Antônio Miranda

    2015-01-01

    Topical therapy is the first choice for the treatment of mild to moderate acne and all-trans retinoic acid is one of the most used drugs. The combination of retinoids and antimicrobials is an innovative approach for acne therapy. Recently, lauric acid, a saturated fatty acid, has shown strong antimicrobial activity against Propionibacterium acnes. However, topical application of retinoic acid is followed by high incidence of side-effects, including erythema and irritation. Solid lipid nanoparticles represent an alternative to overcome these side-effects. This work aims to develop solid lipid nanoparticles loaded with retinoic acid and lauric acid and evaluate their antibacterial activity. The influence of lipophilic stearylamine on the characteristics of solid lipid nanoparticles was investigated. Solid lipid nanoparticles were characterized for size, zeta potential, encapsulation efficiency, differential scanning calorimetry and X-ray diffraction. The in vitro inhibitory activity of retinoic acid-lauric acid-loaded solid lipid nanoparticles was evaluated against Propionibacterium acnes, Staphylococcus aureus and Staphylococcus epidermidis. High encapsulation efficiency was obtained at initial time (94 ± 7% and 100 ± 4% for retinoic acid and lauric acid, respectively) and it was demonstrated that lauric acid-loaded-solid lipid nanoparticles provided the incorporation of retinoic acid. However, the presence of stearylamine is necessary to ensure stability of encapsulation. Moreover, retinoic acid-lauric acid-loaded solid lipid nanoparticles showed growth inhibitory activity against Staphylococcus epidermidis, Propionibacterium acnes and Staphylococcus aureus, representing an interesting alternative for the topical therapy of acne vulgaris. PMID:26328443

  20. Authentication of dried distilled grain with solubles (DDGS) by fatty acid and volatile profiling

    PubMed Central

    Tres, Alba; Heenan, Samuel P.; van Ruth, Saskia

    2014-01-01

    Demand for ethanol substituted fuels from the utilisation of cereal based biofuel has resulted in an over production of dried distillers grains with solubles (DDGS) that are now readily available on the animal feed market. With this rapid emerging availability comes potential variability in the nutritional value of DDGS and possible risks of feed contaminants. Subsequently, the authentication and traceability of alternative animal feed sources is of high priority. In this study and as part of the EU research project “Quality and Safety of Feeds and Food for Europe (QSAFFE FP7-KBBE-2010-4) an attempt was made to classify the geographical origin of cereal grains used in the production of DDGS material. DDGS material of wheat and corn origin were obtained from Europe, China, and the USA. Fatty acid profiles and volatile fingerprints were assessed by gas chromatography flame ionisation (GC-FID) and rapid proton transfer reaction mass spectrometry (PTR-MS) respectively. Chemometric analysis of fatty acid profiles and volatile fingerprints allowed for promising classifications of cereals used in DDGS material by geographical and botanical origin and enabled visual representation of the data. This objective analytical approach could be adapted for routine verification of cereal grains used in the production of DDGS material. PMID:25368433

  1. Fermentation of calcium-fortified soymilk with Lactobacillus: effects on calcium solubility, isoflavone conversion, and production of organic acids.

    PubMed

    Tang, A L; Shah, N P; Wilcox, G; Walker, K Z; Stojanovska, L

    2007-11-01

    The objective of this study was to enhance calcium solubility and bioavailability from calcium-fortified soymilk by fermentation with 7 strains of Lactobacillus, namely, L. acidophilus ATCC 4962, ATCC33200, ATCC 4356, ATCC 4461, L. casei ASCC 290, L. plantarum ASCC 276, and L. fermentum VRI-003. The parameters that were used are viability, pH, calcium solubility, organic acid, and biologically active isoflavone aglycone content. Calcium-fortified soymilk made from soy protein isolate was inoculated with these probiotic strains, incubated for 24 h at 37 degrees C, then stored for 14 d at 4 degrees C. Soluble calcium was measured using atomic absorption spectrophotometry (AA). Organic acids and bioactive isoflavone aglycones, including diadzein, genistein, and glycetein, were measured using HPLC. Viability of the strains in the fermented calcium-fortified soymilk was > 8.5 log(10) CFU/g after 24 h fermentation and this was maintained for 14-d storage at 4 degrees C. After 24 h, there was a significant increase (P < 0.05) in soluble calcium. L. acidophilus ATCC 4962 and L. casei ASCC 290 demonstrated the highest increase with 89.3% and 87.0% soluble calcium after 24 h, respectively. The increase in calcium solubility observed was related to lowered pH associated with production of lactic and acetic acids. Fermentation significantly increased (P < 0.05) the level of conversion of isoflavones into biologically active aglycones, including diadzein, genistein, and glycetein. Our results show that fermenting calcium-fortified soymilk with the selected probiotics can potentially enhance the calcium bioavailability of calcium-fortified soymilk due to increased calcium solubility and bioactive isoflavone aglycone enrichment. PMID:18034738

  2. Formation and catalytic activity of high molecular weight soluble polymers produced by heating amino acids in a modified sea medium

    NASA Astrophysics Data System (ADS)

    Okihana, Hiroyuki

    1982-06-01

    Eighteen protein amino acids with milk casein composition were heated in a modified sea medium. Marigranules were formed in the precipitates and soluble polymers were formed in the supernatant. Time course of the reaction (ultraviolet spectra, the concentration of metal ions, and the concentration of amino acids in the supernatant) were measured. The time course of the formation of the soluble polymers was also studied by Bio-Gel P-2 column. High molecular weight soluble polymers (HMWSP) were separated from low molecular weight ones by dialysis. It was shown that these polymers catalyzed the dehydrogenation of NADH. These polymers also catalyzed the coupled reaction between dehydrogenation of NADH and reduction of resazurin. This coupled reaction was accelerated by the light.

  3. Neopentane and solid acids: direct hydron exchange before cracking.

    PubMed

    Walspurger, Stéphane; Sun, Yinyong; Souna Sido, Abdelkarim Sani; Sommer, Jean

    2006-09-21

    The hydrogen/deuterium exchange reaction of 2,2-dimethylpropane (neopentane) over D(2)O-exchanged zeolites (MOR, FAU, BEA, MFI) using a batch recirculation reactor was studied by means of gas chromatography coupled with mass spectrometer. In the temperature range 473-573 K, H/D exchange proceeds without side reaction such as cracking at short contact times. Indeed the C-H bond has appeared favorably involved in the activation of neopentane compared to the less accessible C-C bond. The transition state allowing hydron exchange is most likely a carbonium species (pentacoordinated carbon) as in the case of the H/D exchange between methane and solid acid. The activation energies of the H/D exchange between neopentane and zeolites are the same for all zeolites indicating a common carbonium ion type transition state. On the basis of previous results in the case of the exchange between methane and liquid superacids, the deuterium exchange rates in neopentane were tentatively related to the acidity of the solids. However the order of activity MOR > MFI > BEA > FAU seems to be related to the size of the pores, which may suggest the involvement of a confinement effect in the zeolites cavities. Moreover we found that H/D exchange takes also place between neopentane and deuterated sulfated zirconia (SZ) emphasizing its strong acidity. PMID:16970460

  4. The participation of soluble factors in the omega-oxidation of fatty acids in the liver of the sheep

    SciTech Connect

    Hare, W.R.; Wahle, K.W. )

    1991-02-01

    The removal of soluble components from an ovine hepatic microsomal preparation decreased the omega-hydroxylation of dodecanoic and hexadecanoic acids. The results suggest that one or more soluble components play a role in the microsomal omega-hydroxylation of fatty acids. The possible roles in the reaction of catalase (known to stimulate the microsomal desaturations of fatty acids and alkylglycerols) and superoxide dismutase were investigated. The addition of these enzymes to the complete (but not the washed) microsomal preparation stimulated both the initial omega-hydroxylation reaction and the subsequent dehydrogenation reactions of the omega-oxidation pathway. The similarity of the effects of catalase and superoxide dismutase and stimulation of two different steps of the omega-oxidation pathway suggest that these agents are acting indirectly by removing active oxygen species rather than directly on the enzymes of microsomal fatty acid omega-hydroxylation.

  5. Effects of soluble ferri-hydroxide complexes on microbial neutralization of acid mine drainage.

    PubMed

    Bilgin, A Azra; Silverstein, JoAnn; Hernandez, Mark

    2005-10-15

    Heterotrophic respiration of ferric iron by Acidiphilium cryptum was investigated in anoxic microcosms with initial media pH values from 1.5 to 3.5. No organic carbon consumption or iron reduction was observed with an initial pH of 1.5, indicating that A. cryptum may not be capable of iron respiration at this pH. Significant iron reduction was observed at pH 2.5 and 3.5, with different effects. When the initial pH was 3.5, pH increased to 4.7-5.5 over 60 days of incubation with simultaneous production of 0.4 g L(-1) Fe2+. However, at an initial pH of 2.5, no significant change in pH was observed during iron respiration, although the accumulation of soluble ferrous iron was significantly higher, averaging 1.1 g L(-1) Fe2+. The speciation of the ferric iron electron acceptor may explain these results. At pH values of 3.5 and higher, precipitated ferric hydroxide Fe- (OH)3 would have been the primary source of ferric iron, with reduction resulting in net production of OH- ions and the significant increases in media pH observed. However at pH 2.5, soluble complexes, FeOH2+ and Fe(OH)2+, may have been the more prevalent electron acceptors, and the alkalinity generated by reduction of complexed iron was low. The existence of charged ferri-hydroxide complexes at pH 2.5 was verified by voltammetry. Results suggest that initiation of bacterial iron reduction may result in neutralization of acid mine drainage. However, this effect is extremely sensitive to iron speciation within a relatively small and critical pH range. PMID:16295843

  6. Efficacy of reducing sugar and phenol-sulfuric acid assays for analysis of soluble carbohydrates in feedstuffs

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Reducing sugar (RSA) and phenol–sulfuric acid (PSA) assays are commonly used to analyze water-soluble carbohydrates. However, questions have arisen as to their accuracy for measurement of feedstuffs with diverse carbohydrate profiles. This study evaluated the efficacy of RSA and PSA as they would co...

  7. Design and validation of software for real-time soluble solids content evaluation of peach by near-infrared spectroscopy

    NASA Astrophysics Data System (ADS)

    Jiang, Minmin; Lu, Huishan; Ying, Yibin; Xu, Huirong

    2006-10-01

    Visible/near infrared spectroscopy on-line determination had been widely used in agricultural products and food samples non-destructive internal quality determination. This research proposed to design real-time determination software in order to estimate soluble solids content (SSC) of fruit on line. Functions of the software included real-time spectroscopy pre-processing, real-time spectroscopy viewing, model building, SSC estimating, etc. In addition, Fenghua juicy peaches were used to validate the practicability and the real-time capability. And SSCs of peach samples were predicted by the software on line. The research provided some help to the real-time non-destructive internal quality determination of the fruit. As the important part of the real-time determination, the determination method and technology were fully accordance with the need at real-time and model's precision.

  8. Quantifying solubility enhancement due to particle size reduction and crystal habit modification: case study of acetyl salicylic acid.

    PubMed

    Hammond, Robert B; Pencheva, Klimentina; Roberts, Kevin J; Auffret, Tony

    2007-08-01

    The poor solubility of potential drug molecules is a significant problem in the design of pharmaceutical formulations. It is well known, however, that the solubility of crystalline materials is enhanced when the particle size is reduced to submicron levels and this factor can be expected to enhance drug product bioavailability. Direct estimation of solubility enhancement, as calculated via the Gibbs-Thompson relationship, demands reasonably accurate values for the particle/solution interfacial tension and, in particular, its anisotropy with respect to the crystal product's habit and morphology. In this article, an improved, more molecule-centered, approach is presented towards the calculation of solubility enhancement factors in which molecular modeling techniques are applied, and the effects associated with both crystal habit modification and solvent choice are examined. A case study for facetted, acetyl salicylic acid (aspirin) crystals in equilibrium with saturated aqueous ethanol solution reveals that their solubility will be enhanced in the range (7-58%) for a crystal size of 0.02 microm, with significantly higher enhancement for crystal morphologies in which the hydrophobic crystal faces are more predominant than the hydrophilic faces and for solvents in which the solubility is smaller. PMID:17323349

  9. Solid state radiolysis of amino acids in an astrochemical perspective

    NASA Astrophysics Data System (ADS)

    Cataldo, Franco; Angelini, Giancarlo; Iglesias-Groth, Susana; Manchado, Arturo

    2011-01-01

    The aliphatic amino acids L-alanine and L-leucine and the aromatic amino acids L-phenylalanine, L-tyrosine and L-tryptophan were irradiated in the solid state to a dose of 3.2 MGy. The degree of decomposition was measured by differential scanning calorimetry (DSC). Furthermore the degree of radioracemization was measured by optical rotatory dispersion (ORD) spectroscopy. From the DSC measurement a radiolysis rate constant k and the half life T1/2 for each amino acid have been determined and extrapolated to a dose of 14 MGy, which corresponds to the expected total dose delivered by the decay of radionuclides to the organic molecules present in comets and asteroids in 4.6×109 years, the age of the Solar System. It is shown that all the amino acids studied can survive a radiation dose of 14 MGy although they are reduced to 1/4-1/5 of their original value they had at the beginning of the history of the Solar System. Consequently, the amount of alanine or leucine found today in the meteorites known as carbonaceous chondrites is just 1/4-1/5 of the amount originally present at the epoch of the formation of the Solar System 4.6×109 years ago. Among the amino acids studied, tyrosine shows the highest radiation resistance while tryptophan does not combine its relatively high radiation resistance with an elevated level of radioracemization resistance. Apart from the exception of tryptophan, it is shown that the radiolysis rate constants k of all the amino acids studied are in reasonable agreement with the radioracemization rate constant krac.

  10. Vibrational entropy changes the solid solubility of a random alloy at high temperatures

    NASA Astrophysics Data System (ADS)

    Shulumba, Nina; Hellman, Olle; Raza, Zamaan; Barrirero, Jenifer; Mücklich, Frank; Abrikosov, Igor A.; Odén, Magnus

    2015-03-01

    We have developed a method to accurately and efficiently determine vibrational entropy as a function of temperature and volume for substitutional alloys from first principles. Using Ti1-xAlxN metal alloy as a model system we calculate the isostructural phase diagram by minimization of the free energy, solving the original Gibbs problem of finding its global minimum corresponding to the true equilibrium state of the system. We demonstrate that the vibrational contribution to the free energy has a decisive impact on the calculated phase diagram of Ti1-xAlxN alloy, lowering the maximum temperature for the miscibility gap from 9000 K to 2400 K. The solubility limit of the predicted phase diagram is experimentally verified by local chemical composition measurements of thermally aged Ti50Al50N alloys. DocMASE, SECO Tools AB, SSF RMA 08-0069 and SRL 10-002, VR 2012-4401 and 637-2013-7296, Vinnova M-ERA.net, MC2, (KAW) (Isotopic Control for Ultimate Material Properties).

  11. Relative effectiveness of various anions on the solubility of acidic Hypoderma lineatum collagenase at pH 7.2.

    PubMed Central

    Carbonnaux, C.; Ries-Kautt, M.; Ducruix, A.

    1995-01-01

    The effects of various anions on decreasing the solubility of acidic Hypoderma lineatum collagenase at pH 7.2 and 18 degrees C were qualitatively defined by replacing the crystallizing agent of known crystallization conditions by various ammonium salts. The solubility curves measured in the presence of the sulfate, phosphate, citrate, and chloride ammonium salts gave the following ranking of anions: HPO4(2-)/H2PO4- > SO4(2-) > citrate 3-/citrate2- >> Cl-. This order is in agreement with the Hofmeister series. In a previous study on the solubility at pH 4.5 of lysozyme, a basic protein, the effectiveness of anions in decreasing the solubility was found to be in the reverse order. This suggests that the effectiveness of anions in the crystallization of proteins is dependent on the net charge of the protein, i.e., depending on whether a basic protein is crystallized at acidic pH or an acidic protein at basic pH. PMID:8535249

  12. Design, synthesis, structure, and dehydrogenation reactivity of a water-soluble o-iodoxybenzoic acid derivative bearing a trimethylammonium group.

    PubMed

    Cui, Li-Qian; Dong, Zhi-Lei; Liu, Kai; Zhang, Chi

    2011-12-16

    5-Trimethylammonio-1,3-dioxo-1,3-dihydro-1λ(5)-benzo[d][1,2]iodoxol-1-ol anion (AIBX 1a), an o-iodoxybenzoic acid (IBX) derivative having the trimethylammonium moiety on its phenyl ring, possesses very good solubility in water and distinct oxidative properties from IBX, which is demonstrated in the oxidation of various β-keto esters to the corresponding dehydrogenated products using water as cosolvent. The regeneration of AIBX 1a can be easily realized from the reaction mixture due to its good water solubility. PMID:22082110

  13. [Effects of simulated acid rain and its acidified soil on soluble sugar and nitrogen contents of wheat seedlings].

    PubMed

    Tong, Guanhe; Liang, Huiling

    2005-08-01

    The study showed that the cation release of simulated rain caused soil acidification and base ions release. With the decrease of simulated acid rain pH from 5.6 to 2.5, the acid rain-leached soil pH decreased from 6.06 to 3.41, and its total amount of exchange base ions decreased from 56.5 to 41.1 mmol x kg(-1). Spraying simulated acid rain on the shoots of wheat seedlings planted on such acidified soils caused a rapid decrease in the soluble sugar and nitrogen contents of wheat seedlings, and reduced some of their physiological activities. The effect of spraying simulated acid rain on the soluble sugar, nitrogen, and chlorophyll contents and photosynthetic rate of wheat stems and leaves was larger than that of acidified soil, while the effect of the latter on the soluble sugar and nitrogen contents and the physiological activity of NR and GOGAT in root system of wheat seedlings was larger than that of the former. The intensive acid rain of pH < or = 3.0 and the corresponding acidified soil had an obvious harm to the growth and physiological activity of wheat seedlings. PMID:16262064

  14. Enhancement of the water solubility of organic pollutants such as pyrene and atrazine by dissolved humic and fulvic acids

    SciTech Connect

    Patterson, H.H.; MacDonald, B.; Fang, F.

    1995-12-31

    Many factors determine the fate and transport of an organic pollutant in the environment but water solubility is certainly one of the most important. Among the environmental factors that alter the solubility of a molecule are naturally occurring humic and fulvic acids. We have hypothesized that the humic/fulvic acids from different sources within a watershed have different binding affinities for pollutants such as pyrene and atrazine. This could lead to different rates of transport or bioavailability within the watershed. Humic/fulvic acids were isolated from a stream, adjacent wetland and nearby wooded upland sites. A fluorescence quenching method was developed to quantify the binding coefficient of the pollutants with the dissolved organic carbon. From these results a model was constructed to determine the sites with the greatest potential to modify pollutant contamination in the environment.

  15. Highly water-soluble mast cell stabiliser-encapsulated solid lipid nanoparticles with enhanced oral bioavailability.

    PubMed

    Patel, Ravi R; Chaurasia, Sundeep; Khan, Gayasuddin; Chaubey, Pramila; Kumar, Nagendra; Mishra, Brahmeshwar

    2016-05-01

    Cromolyn sodium (CS), a mast cell stabiliser, is widely employed for the prevention and treatment of allergic conditions. However, high hydrophilicity and poor oral permeability hinder its oral clinical translation. Here, solid lipid nanoparticles (SLNs) have been developed for the purpose of oral bioavailability enhancement. The CS-SLNs were engineered by double emulsification method (W1/O/W2) and optimised by using Box-Behnken experimental design. The surface and solid-state characterisations revealed the presence of CS in an amorphous form without any interactions inside the spherical-shaped SLNs. The in-vitro release study showed an extended release up to 24 hr by diffusion controlled process. Ex-vivo and in-vivo intestinal permeation study showed ∼2.96-fold increase in permeability of CS by presentation as SLNs (p < 0.05). Further, in-vivo pharmacokinetic study exhibited ∼2.86-fold enhancements in oral bioavailability of CS by encapsulating inside SLNs, which clearly indicate that SLNs can serve as the potential therapeutic carrier system for oral delivery of CS. PMID:26885889

  16. Identification of a Soluble, High-Affinity Salicylic Acid-Binding Protein in Tobacco.

    PubMed Central

    Du, H.; Klessig, D. F.

    1997-01-01

    Salicylic acid (SA) is a key component in the signal transduction pathway(s), leading to the activation of certain defense responses in plants after pathogen attack. Previous studies have identified several proteins, including catalase and ascorbate peroxidase, through which the SA signal might act. Here we describe a new SA-binding protein. This soluble protein is present in low abundance in tobacco (Nicotiana tabacum) leaves and has an apparent molecular weight of approximately 25,000. It reversibly binds SA with an apparent dissociation constant of 90 nM, an affinity that is 150-fold higher than that between SA and catalase. The ability of most analogs of SA to compete with labeled SA for binding to this protein correlated with their ability to induce defense gene expression and enhanced resistance. Strikingly, benzothiadiazole, a recently described chemical activator that induces plant defenses and disease resistance at very low rates of application, was the strongest competitor, being much more effective than unlabeled SA. The possible role of this SA-binding protein in defense signal transduction is discussed. PMID:12223676

  17. Influence of acid-soluble proteins from bivalve Siliqua radiata ligaments on calcium carbonate crystal growth

    NASA Astrophysics Data System (ADS)

    Huang, Zeng-Qiong; Zhang, Gang-Sheng

    2016-08-01

    In vitro biomimetic synthesis of calcium carbonate (CaCO3) in the presence of shell proteins is a heavily researched topic in biomineralization. However, little is known regarding the function of bivalve ligament proteins in the growth of CaCO3 crystals. In this study, using fibrous protein K58 from Siliqua radiata ligaments or coverslips as substrates, we report the results of our study of CaCO3 precipitation in the presence or absence of acid-soluble proteins (ASP) from inner ligament layers. ASP can disturb the controlling function of K58 or a coverslip on the crystalline phase, resulting in the formation of aragonite, calcite, and vaterite. In addition, we identified the following four primary components from ASP by mass spectroscopy: alkaline phosphatase (ALP), ABC transporter, keratin type II cytoskeletal 1 (KRT 1), and phosphate ABC transporter, phosphate-binding protein (PstS). Further analysis revealed that the first three proteins and especially ALP, which is important in bone mineralisation, could affect the polymorphism and morphology of CaCO3 crystals by trapping calcium ions in their domains. Our results indicate that ALP may play an important role in the formation of aragonite in S. radiata ligaments. This paper may facilitate our understanding of the biomineralization process.

  18. Characterisation of acid-soluble and pepsin-solubilised collagen from jellyfish (Cyanea nozakii Kishinouye).

    PubMed

    Zhang, Junjie; Duan, Rui; Huang, Lei; Song, Yujie; Regenstein, Joe M

    2014-05-01

    Annual outbreaks of the Jellyfish (Cyanea nozakii Kishinouye) in the waters of the Yellow Sea and the East China Sea are regarded as a nuisance. Thus, utilizing this jellyfish species is of great significance to reduce harm to fisheries and marine environments. The yield of the acid-soluble collagens (ASCs) from the C. nozakii umbrella was 13.0% (dry weight) and that of the pepsin-solubilised collagens (PSCs) was 5.5% (dry weight). The SDS-PAGE patterns of the ASCs and PSCs differed from that of type I collagen, which indicate the presence of (α1)3. The denaturation temperature (Td) of the collagens was approximately 23.8°C. Fourier transform infrared spectroscopy proved that the ASCs and PSCs retained their helical structures and the As, Pb, and Hg content of the collagens, detected by ICP-MS, were considerably lower than the national standards. The results suggest that collagens isolated from C. nozakii can potentially be used as an alternative source of collagen for use in various applications. PMID:24360414

  19. Adsorption and condensation of amino acids and nucleotides with soluble mineral salts

    NASA Technical Reports Server (NTRS)

    Orenberg, J.; Lahav, N.

    1986-01-01

    The directed synthesis of biopolymers in an abiotic environment is presumably a cyclic sequence of steps which may be realized in a fluctuating environment such as a prebiotic pond undergoing wetting-drying cycles. Soluble mineral salts have been proposed as an essential component of this fluctuating environment. The following sequence may be considered as a most primitive mechanism of information transfer in a fluctuating environment: (1) adsorption of a biomolecule onto a soluable mineral salt surface to act as an adsorbed template; (2) specific adsorption of biomonomers onto the adsorbed template; (3) condensation of the adsorbed biomonomers; and (4) desorption of the elongated oligomer. In this investigation, the salts selected for study were CaSO4.2H2O(gypsum), SrSO4, and several other metal sulfates and chlorides. Adsorption of the monomeric species, gly, 5'AMP 5'GMP, and 5'CMP was investigated. The adsorbed template biopolymers used were Poly-A, Poly-G, Poly-C, and Poly-U. The results of studies involving these experimental participants, the first two steps of the proposed primitive information transfer mechanism, and condensation of amino acids to form oligomers in a fluctuating environment are to be reported.

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

    PubMed Central

    Singh, Jatinderpal; Garg, Rajeev; Gupta, Ghanshyam Das

    2015-01-01

    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. PMID:26634173

  1. Solid dispersion of quercetin in cellulose derivative matrices influences both solubility and stability.

    PubMed

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

    2013-02-15

    Amorphous solid dispersions (ASD) of quercetin (Que) in cellulose derivative matrices, carboxymethylcellulose acetate butyrate (CMCAB), hydroxypropylmethylcellulose acetate succinate (HPMCAS), and cellulose acetate adipate propionate (CAAdP) were prepared with the goal of identifying an ASD that effectively increased Que aqueous solution concentration. Crystalline quercetin and Que/poly(vinylpyrrolidinone) (PVP) ASD were evaluated for comparison. Powder X-ray diffraction (XRPD) and differential scanning calorimetry (DSC) were used to examine the crystallinity of ASDs, physical mixtures (PM) and quercetin. ASDs were amorphous up to 50 wt% Que. Que stability against crystallization and solution concentrations from these ASDs were significantly higher than those observed for physical mixtures and crystalline Que. PVP stabilizes against both Que degradation and recrystallization; in contrast, these carboxylated cellulose derivatives inhibit recrystallization but release Que slowly. PVP ASDs afforded fast and complete drug release, while ASDs using these three cellulose derivatives provide slow, incomplete, pH-triggered drug release. PMID:23399255

  2. Impact of fresh and composted solid olive husk and their water-soluble fractions on soil heavy metal fractionation; microbial biomass and plant uptake.

    PubMed

    de la Fuente, Carlos; Clemente, Rafael; Martínez-Alcalá, Isabel; Tortosa, Germán; Bernal, M Pilar

    2011-02-28

    The use of waste materials as organic amendments in soil remediation can affect metal solubility; this interaction will vary with the characteristics of the organic matter that is added to the soil. A pot experiment was carried out in a calcareous, metal-polluted soil, using Beta maritima L. as an indicator species for the treatment effects on metal solubility. The treatments were: fresh solid olive husk, a mature compost, their respective water extracts (as the most reactive and biodegradable fraction) and an unamended, control soil. The compost reduced metal availability and plant uptake, while fresh olive husk favoured Mn bioavailability and produced phytotoxicity. The water-soluble extract from fresh solid olive husk also provoked elevated Mn solubility in soil, but did not increase Mn uptake by plants. The application of water-soluble organic matter obtained from compost did not affect heavy metal solubility significantly. Therefore, composted olive husk seems to be the most-appropriate material for the development of bioremediation strategies. PMID:21216095

  3. Purified membrane and soluble folate binding proteins from cultured KB cells have similar amino acid compositions and molecular weights but differ in fatty acid acylation.

    PubMed Central

    Luhrs, C A; Pitiranggon, P; da Costa, M; Rothenberg, S P; Slomiany, B L; Brink, L; Tous, G I; Stein, S

    1987-01-01

    A membrane-associated folate binding protein (FBP) and a soluble FBP, which is released into the culture medium, have been purified from human KB cells using affinity chromatography. By NaDodSO4/PAGE, both proteins have an apparent Mr of approximately 42,000. However, in the presence of Triton X-100, the soluble FBP eluted from a Sephadex G-150 column with an apparent Mr of approximately 40,000 (similar to NaDodSO4/PAGE) but the membrane-associated FBP eluted with an apparent Mr of approximately 160,000, indicating that this species contains a hydrophobic domain that interacts with the detergent micelles. The amino acid compositions of both forms of FBP were similar, especially with respect to the apolar amino acids. In addition, the 18 amino acids at the amino termini of both proteins were identical. The membrane FBP, following delipidation with chloroform/methanol, contained 7.1 mol of fatty acid per mol of protein, of which 4.7 mol was amide-linked and 2.4 mol was ester-linked. The soluble FBP contained only 0.05 mol of fatty acid per mol of protein. These studies indicate that the membrane FBP of KB cells contains covalently bound fatty acids that may serve to anchor the protein in the cell membrane. Images PMID:3476960

  4. Removal and recovery of furfural, 5-hydroxymethylfurfural, and acetic acid from aqueous solutions using a soluble polyelectrolyte.

    PubMed

    Carter, Brian; Gilcrease, Patrick C; Menkhaus, Todd J

    2011-09-01

    In the cellulosic ethanol process, furfural, 5-hydroxymethylfurfural (HMF), and acetic acid are formed during the high temperature acidic pretreatment step needed to convert biomass into fermentable sugars. These compounds can inhibit cellulase enzymes and fermentation organisms at relatively low concentrations (≥ 1 g/L). Effective removal of these inhibitory compounds would allow the use of more severe pretreatment conditions to improve sugar yields and lead to more efficient fermentations; if recovered and purified, they could also be sold as valuable by-products. This study investigated the separation of aldhehydes (furfural and HMF) and organic acid (acetic acid) inhibitory compounds from simple aqueous solutions by using polyethyleneimene (PEI), a soluble cationic polyelectrolyte. PEI added to simple solutions of each inhibitor at a ratio of 1 mol of functional group to 1 mol inhibitor removed up to 89.1, 58.6, and 81.5 wt% of acetic acid, HMF, and furfural, respectively. Furfural and HMF were recovered after removal by washing the polyelectrolyte/inhibitor complex with dilute sulfuric acid solution. Recoveries up to 81.0 and 97.0 wt% were achieved for furfural and HMF, respectively. The interaction between PEI and acetic acid was easily disrupted by the addition of chloride ions, sulfate ions, or hydroxide ions. The use of soluble polymers for the removal and recovery of inhibitory compounds from biomass slurries is a promising approach to enhance the efficiency and economics of an envisioned biorefinery. PMID:21455937

  5. Improved Release of Celecoxib from High Drug Loading Amorphous Solid Dispersions Formulated with Polyacrylic Acid and Cellulose Derivatives.

    PubMed

    Xie, Tian; Taylor, Lynne S

    2016-03-01

    Amorphous solid dispersions (ASDs) have been extensively exploited as a strategy for improving the dissolution performance of poorly water-soluble drugs. However, factors underpinning the observed dissolution profiles are not clearly understood, and the choice of polymeric carriers is largely empirical. In the current study, the dissolution performance of a high drug loading ASD containing the poorly water-soluble, anti-inflammatory agent, celecoxib, was optimized by using binary polymers combinations. Polyacrylic acid (PAA), a highly water-soluble polymer, was used to substantially increase the dissolution rate of the drug, while hydroxypropyl methyl cellulose (HPMC) or HPMC acetate succinate (HPMCAS) were added to stabilize the solid amorphous matrix against crystallization upon hydration, as well as to maintain supersaturation. Quantitative measurements of the impact of the polymers on the solution nucleation and growth rates of celecoxib revealed that, while the cellulose derivatives are effective nucleation inhibitors, it is more difficult to completely prevent crystal growth in solutions containing seed crystals, in particular at high supersaturations. Therefore, it is critical to prevent the formation of crystals in the dissolving matrix during dissolution. By using certain ratios of HPMC and PAA, both rapid release as well as crystallization inhibition could be achieved, even at high drug loadings. Utilizing combinations of polymers may therefore be useful to tailor release profiles while providing optimized crystallization inhibition. PMID:26791934

  6. Soluble epoxide hydrolase contamination of specific catalase preparations inhibits epoxyeicosatrienoic acid vasodilation of rat renal arterioles.

    PubMed

    Gauthier, Kathryn M; Olson, Lauren; Harder, Adam; Isbell, Marilyn; Imig, John D; Gutterman, David D; Falck, J R; Campbell, William B

    2011-10-01

    Cytochrome P-450 metabolites of arachidonic acid, the epoxyeicosatrienoic acids (EETs) and hydrogen peroxide (H(2)O(2)), are important signaling molecules in the kidney. In renal arteries, EETs cause vasodilation whereas H(2)O(2) causes vasoconstriction. To determine the physiological contribution of H(2)O(2), catalase is used to inactivate H(2)O(2). However, the consequence of catalase action on EET vascular activity has not been determined. In rat renal afferent arterioles, 14,15-EET caused concentration-related dilations that were inhibited by Sigma bovine liver (SBL) catalase (1,000 U/ml) but not Calbiochem bovine liver (CBL) catalase (1,000 U/ml). SBL catalase inhibition was reversed by the soluble epoxide hydrolase (sEH) inhibitor tAUCB (1 μM). In 14,15-EET incubations, SBL catalase caused a concentration-related increase in a polar metabolite. Using mass spectrometry, the metabolite was identified as 14,15-dihydroxyeicosatrienoic acid (14,15-DHET), the inactive sEH metabolite. 14,15-EET hydrolysis was not altered by the catalase inhibitor 3-amino-1,2,4-triazole (3-ATZ; 10-50 mM), but was abolished by the sEH inhibitor BIRD-0826 (1-10 μM). SBL catalase EET hydrolysis showed a regioisomer preference with greatest hydrolysis of 14,15-EET followed by 11,12-, 8,9- and 5,6-EET (V(max) = 0.54 ± 0.07, 0.23 ± 0.06, 0.18 ± 0.01 and 0.08 ± 0.02 ng DHET·U catalase(-1)·min(-1), respectively). Of five different catalase preparations assayed, EET hydrolysis was observed with two Sigma liver catalases. These preparations had low specific catalase activity and positive sEH expression. Mass spectrometric analysis of the SBL catalase identified peptide fragments matching bovine sEH. Collectively, these data indicate that catalase does not affect EET-mediated dilation of renal arterioles. However, some commercial catalase preparations are contaminated with sEH, and these contaminated preparations diminish the biological activity of H(2)O(2) and EETs. PMID:21753077

  7. Measurement of moisture, soluble solids, and sucrose content and mechanical properties in sugar beet using portable visible and near-infrared spectroscopy

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Visible and near-infrared spectroscopy, coupled with partial least squares regression, was used to predict the moisture, soluble solids and sucrose content and mechanical properties of sugar beet. Interactance spectra were acquired from both intact and sliced beets, using two portable spectrometers ...

  8. Interactions between water soluble porphyrin-based star polymer and amino acids: Spectroscopic evidence of molecular binding

    NASA Astrophysics Data System (ADS)

    Angelini, Nicola; Micali, Norberto; Villari, Valentina; Mineo, Placido; Vitalini, Daniele; Scamporrino, Emilio

    2005-02-01

    Molecular interactions giving rise to stable complexes between an uncharged water soluble cobalt-porphyrin and amino acids are investigated by time-resolved fluorescence, uv-vis, and circular dichroism measurements. This metalloporphyrin seems to act, by means of the coordination site of the cobalt of the core, as a recognition host, preferentially, with amino acids possessing aromatic groups. The binding with aliphatic amino acids requires longer time scales to be efficient and likely involves a slow kinetic process. The experimental findings suggest that, besides the metal(host)-N(guest) coordination bond, which is the common requisite for all amino acids, a preferential interaction with aromatic groups exists there. The solubility in water of the molecule, guaranteed by the polyethylene glycol arms as peripheral substituents, in the absence of electric charges, allows for a more selective discrimination of the binding process with respect to other water-soluble charged porphyrins. The interest devoted to the porphyrin-based star polymer and its recognition properties is, therefore, founded on the potential use either in polymeric matrices for material science or in aqueous solution for bioscience.

  9. Prevention of Acid Mine Drainage Through Complexation of Ferric Iron by Soluble Microbial Growth Products

    NASA Astrophysics Data System (ADS)

    Pandey, S.; Yacob, T. W.; Silverstein, J.; Rajaram, H.; Minchow, K.; Basta, J.

    2011-12-01

    Acid mine drainage (AMD) is a widespread environmental problem with deleterious impacts on water quality in streams and watersheds. AMD is generated largely by the oxidation of metal sulfides (i.e. pyrite) by ferric iron. This abiotic reaction is catalyzed by conversion of ferrous to ferric iron by iron and sulfur oxidizing microorganisms. Biostimulation is currently being investigated as an attempt to inhibit the oxidation of pyrite and growth of iron oxidizing bacteria through addition of organic carbon. This may stimulate growth of indigenous communities of acidophilic heterotrophic bacteria to compete for oxygen. The goal of this research is to investigate a secondary mechanism associated with carbon addition: complexation of free Fe(III) by soluble microbial growth products (SMPs) produced by microorganisms growing in waste rock. Exploratory research at the laboratory scale examined the effect of soluble microbial products (SMPs) on the kinetics of oxidation of pure pyrite during shaker flask experiments. The results confirmed a decrease in the rate of pyrite oxidation that was dependent upon the concentration of SMPs in solution. We are using these data to verify results from a pyrite oxidation model that accounts for SMPs. This reactor model involves differential-algebraic equations incorporating total component mass balances and mass action laws for equilibrium reactions. Species concentrations determined in each time step are applied to abiotic pyrite oxidation rate expressions from the literature to determine the evolution of total component concentrations. The model was embedded in a parameter estimation algorithm to determine the reactive surface area of pyrite in an abiotic control experiment, yielding an optimized value of 0.0037 m2. The optimized model exhibited similar behavior to the experiment for this case; the root mean squared of residuals for Fe(III) was calculated to be 7.58 x 10-4 M, which is several orders of magnitude less than the actual

  10. Characterization of acid-and pepsin-soluble collagens from spines and skulls of skipjack tuna (Katsuwonus pelamis).

    PubMed

    Yu, Di; Chi, Chang-Feng; Wang, Bin; Ding, Guo-Fang; Li, Zhong-Rui

    2014-09-01

    Acid-soluble collagen (ASC) and pepsin-soluble collagen (PSC) from the spine (ASC-SP and PSC-SP) and skull (ASC-SK and PSC-SK) of the skipjack tuna, Katsuwonus pelamis, were successfully isolated and characterized. The yields of ASC-SP, PSC-SP, ASC-SK and PSC-SK were (2.47 ± 0.39)%, (5.62 ± 0.82)%, (3.57 ± 0.40)%, and (6.71 ± 0.81)%, respectively, on the basis of dry weight. The four collagens contained Gly (330.2-339.1 residues/1 000 residues) as the major amino acid, and their imino acid contents were between 168.8 and 178.2 residues/1 000 residues. Amino acid composition, SDS-PAGE, and FTIR investigations confirmed that ASC-SP and ASC-SK were mainly composed of type I collagen, and had higher contents of high-molecular weight cross-links than those of PSC-SK and PSC-SP. The FTIR investigation also certified all the collagens had triple helical structure. The denaturation temperatures of ASC-SK, PSC-SK, ASC-SP, and PSC-SP were 17.8, 16.6, 17.6, and 16.5 °C, respectively. All isolated collagens were soluble at acidic pH (1-5) and lost their solubilities when the NaCl concentration was above 2% (W/V). The isolated collagens from the spines and skulls of skipjack tuna could serve as an alternative source of collagens for further application in food, cosmetic, biomedical, and pharmaceutical industries. PMID:25263986

  11. A review on synthesis and characterization of solid acid materials for fuel cell applications

    NASA Astrophysics Data System (ADS)

    Mohammad, Norsyahida; Mohamad, Abu Bakar; Kadhum, Abdul Amir H.; Loh, Kee Shyuan

    2016-08-01

    Solid acids emerged as an electrolyte material for application in fuel cells due to their high protonic conductivity and stability at high temperatures between 100 °C and 250 °C. This paper gives an overview of the different solid acid materials and their properties, such as high protonic conductivity and thermal stability, in relation to phase transitions and mechanisms of proton transport. Various solid acid synthesis methods including aqueous and dry mixing, electrospinning, sol-gel, impregnation and thin-film casting will be discussed, and the impact of synthesis methods on the properties of solid acids will be highlighted. The properties of solid acids synthesized as either single crystals and or polycrystalline powders were identified via X-ray diffraction, nuclear magnetic resonance, thermal analyses, optical microscopy and infrared spectroscopy. A selection of electrolyte-electrode assembly methods and the performance of solid acid fuel cell prototypes are also reviewed.

  12. Dissolution Profile of Mefenamic Acid Solid Dosage Forms in Two Compendial and Biorelevant (FaSSIF) Media.

    PubMed

    Nurhikmah, Wilda; Sumirtapura, Yeyet Cahyati; Pamudji, Jessie Sofia

    2016-01-01

    Mefenamic acid is a non-steroidal anti-inflammatory drug (NSAID) that is widely used for the treatment of mild-to-moderate pain. Mefenamic acid belongs to the Biopharmaceutical Classification System (BCS) class II drug which has lower water solubility but high permeability. There are two different compendial methods available for dissolution tests of mefenamic acid solid dosage forms, i.e. methods of United States Pharmacopeia 37 (USP) and Pharmacopoeia of the People's Republic of China 2010 (PPRC). Indonesian Pharmacopeia V ed. (FI) adopted the USP method. On the other hand, many researches focused on the use of a 'biorelevant' medium to develop the dissolution test method. The aim of this research was to study the dissolution profile of mefenamic acid from its solid dosage forms (caplet and capsule) available in the Indonesian market with three different dissolution medium: USP, PPRC, and biorelevant fasted simulated small intestinal fluid (FaSSIF) media. The tested products consisted of the innovator's product (available only in caplet dosage form, FN caplet) and generic products (available as caplet and capsule). The dissolution test of the drug products in all dissolution media was performed in 900 mL of medium using apparatus II (paddle) at a temperature of 37°C and rotation speed of 75 rpm, except for the capsule product and for USP medium, both of which tests were done using apparatus I (basket) with rotation speed of 100 rpm. The solubility test of mefenamic acid was carried out in all media at temperature of 37°C. The result obtained from the solubility test showed that the the highest solubility of mefenamic acid was obtained in USP medium (approximately 2 mg/mL), followed by PPRC medium (about 0.5 mg/mL), and FaSSIF medium (approximately 0.06 mg/ml). In the dissolution test, percentage of drug dissolved in in the USP and PPRC media after 45 min for all products reached more than 75%, except for the PN caplet in USP medium which reached only about 44

  13. Dissolution Profile of Mefenamic Acid Solid Dosage Forms in Two Compendial and Biorelevant (FaSSIF) Media

    PubMed Central

    Nurhikmah, Wilda; Sumirtapura, Yeyet Cahyati; Pamudji, Jessie Sofia

    2016-01-01

    Mefenamic acid is a non-steroidal anti-inflammatory drug (NSAID) that is widely used for the treatment of mild-to-moderate pain. Mefenamic acid belongs to the Biopharmaceutical Classification System (BCS) class II drug which has lower water solubility but high permeability. There are two different compendial methods available for dissolution tests of mefenamic acid solid dosage forms, i.e. methods of United States Pharmacopeia 37 (USP) and Pharmacopoeia of the People’s Republic of China 2010 (PPRC). Indonesian Pharmacopeia V ed. (FI) adopted the USP method. On the other hand, many researches focused on the use of a ‘biorelevant’ medium to develop the dissolution test method. The aim of this research was to study the dissolution profile of mefenamic acid from its solid dosage forms (caplet and capsule) available in the Indonesian market with three different dissolution medium: USP, PPRC, and biorelevant fasted simulated small intestinal fluid (FaSSIF) media. The tested products consisted of the innovator’s product (available only in caplet dosage form, FN caplet) and generic products (available as caplet and capsule). The dissolution test of the drug products in all dissolution media was performed in 900 mL of medium using apparatus II (paddle) at a temperature of 37°C and rotation speed of 75 rpm, except for the capsule product and for USP medium, both of which tests were done using apparatus I (basket) with rotation speed of 100 rpm. The solubility test of mefenamic acid was carried out in all media at temperature of 37°C. The result obtained from the solubility test showed that the the highest solubility of mefenamic acid was obtained in USP medium (approximately 2 mg/mL), followed by PPRC medium (about 0.5 mg/mL), and FaSSIF medium (approximately 0.06 mg/ml). In the dissolution test, percentage of drug dissolved in in the USP and PPRC media after 45 min for all products reached more than 75%, except for the PN caplet in USP medium which reached only

  14. Understanding Particle Formation: Solubility of Free Fatty Acids as Polysorbate 20 Degradation Byproducts in Therapeutic Monoclonal Antibody Formulations.

    PubMed

    Doshi, Nidhi; Demeule, Barthélemy; Yadav, Sandeep

    2015-11-01

    The purpose of this work was to determine the aqueous solubilities at 2-8 °C of the major free fatty acids (FFAs) formed by polysorbate 20 (PS20) degradation and identify possible ways to predict, delay, or mitigate subsequent particle formation in monoclonal antibody (mAb) formulations. The FFA solubility limits at 2-8 °C were determined by titrating known amounts of FFA in monoclonal antibody formulations and identifying the FFA concentration leading to visible and subvisible particle formation. The solubility limits of lauric, myristic, and palmitic acids at 2-8 °C were 17 ± 1 μg/mL, 3 ± 1 μg/mL, and 1.5 ± 0.5 μg/mL in a formulation containing 0.04% (w/v) PS20 at pH 5.4 and >22 μg/mL, 3 ± 1 μg/mL, and 0.75 ± 0.25 μg/mL in a formulation containing 0.02% (w/v) PS20 at pH 6.0. For the first time, a 3D correlation between FFA solubility, PS20 concentration, and pH has been reported providing a rational approach for the formulator to balance these with regard to potential particle formation. The results suggest that the lower solubilities of the longer chain FFAs, generated from degradation of the stearate, palmitate, and myristate fraction of PS20, is the primary cause of seeding and subsequent FFA precipitation rather than the most abundant lauric acid. PMID:26419285

  15. Using the concept of Chou's pseudo amino acid composition to predict protein solubility: an approach with entropies in information theory.

    PubMed

    Xiaohui, Niu; Nana, Li; Jingbo, Xia; Dingyan, Chen; Yuehua, Peng; Yang, Xiao; Weiquan, Wei; Dongming, Wang; Zengzhen, Wang

    2013-09-01

    Protein solubility plays a major role and has strong implication in the proteomics. Predicting the propensity of a protein to be soluble or to form inclusion body is a fundamental and not fairly resolved problem. In order to predict the protein solubility, almost 10,000 protein sequences were downloaded from NCBI. Then the sequences were eliminated for the high homologous similarity by CD-HIT. Thus, there were 5692 sequences remained. Based on protein sequences, amino acid and dipeptide compositions were generally extracted to predict protein solubility. In this study, the entropy in information theory was introduced as another predictive factor in the model. Experiments involving nine different feature vector combinations, including the above-mentioned three kinds of factors, were conducted with support vector machines (SVMs) as prediction engine. Each combination was evaluated by re-substitution test and 10-fold cross-validation test. According to the evaluation results, the accuracies and Matthew's Correlation Coefficient (MCC) values were boosted by the introduction of the entropy. The best combination was the one with amino acid, dipeptide compositions and their entropies. Its accuracy reached 90.34% and Matthew's Correlation Coefficient (MCC) value was 0.7494 in re-substitution test, while 88.12% and 0.7945 respectively for 10-fold cross-validation. In conclusion, the introduction of the entropy significantly improved the performance of the predictive method. PMID:23524162

  16. The Effect of Supercritical Fluids on Solid Acid Catalyst Alkylation

    SciTech Connect

    Ginosar, Daniel Michael; Thompson, David Neil; Burch, Kyle Coates; Zalewski, D. J.

    2002-05-01

    The alkylation of isobutane with trans-2-butene was explored over six solid acid catalysts in the liquid, near-critical liquid, and supercritical regions through the addition of an inert cosolvent to the reaction feed mixture. The addition of supercritical cosolvents did not result in sustained catalytic alkylation activity. A modest improvement in product yield was obtained with the addition of methane in the modified-liquid region; however, catalyst longevity and product selectivity were decreased compared to cosolvent-free liquid conditions. This paper describes the catalyst screening and selection process, an exploration of catalyst performance with varying concentrations of methane, and an examination of the effects of seven supercritical fluids on catalyst performance. The catalysts included two zeolites, two sulfated metal oxides, and two Nafion catalysts. Three hydrocarbons, two fluorocarbons, carbon dioxide, and sulfur hexafluoride were explored as inert cosolvents added to the reaction mixture.

  17. Development of clinical dosage forms for a poorly water soluble drug I: Application of polyethylene glycol-polysorbate 80 solid dispersion carrier system.

    PubMed

    Dannenfelser, Rose-Marie; He, Handan; Joshi, Yatindra; Bateman, Simon; Serajuddin, Abu T M

    2004-05-01

    Different formulation approaches were evaluated to ensure that the formulation of a poorly water soluble compound chosen during early development achieves optimum bioavailability. The insoluble compound has an aqueous solubility of 0.17 micro g/mL at 25 +/- 1 degrees C, a relatively high permeability (Caco2 P(app) = 6.1 x 10(-4) cm/min), and poor bioavailability in dogs (dry blend formulation). Based on the prediction by GastroPlus, the oral absorption of this compound is sensitive to its apparent solubility and particle size. The oral bioavailability of three different formulations was compared in a dog model: a cosolvent-surfactant solution, a solid dispersion in a mixture of polyethylene glycol 3350 and polysorbate 80, and a dry blend of micronized drug with microcrystalline cellulose. In absence of a parenteral injection, the bioavailability of the solution was considered to be 100%, and the relative oral bioavailability of the three formulations was 100, 99.1, 9.8, respectively. Comparable bioavailability was obtained with the solid dispersion and the cosolvent-surfactant solution, both of which showed a 10-fold higher bioavailability than the dry blend. Thus, a 20 mg dose strength capsule containing the solid dispersion formulation was selected for clinical development. The selected solid dispersion system was physically and chemically stable for at least 16 months at 25 degrees C/60% RH. In conclusion, the bioavailability of a poorly water soluble drug was greatly enhanced using the solid dispersion formulation containing a water soluble polymer with a surface active agent. PMID:15067693

  18. Restoration of Brain Acid Soluble Protein 1 Inhibits Proliferation and Migration of Thyroid Cancer Cells

    PubMed Central

    Guo, Run-Sheng; Yu, Yue; Chen, Jun; Chen, Yue-Yu; Shen, Na; Qiu, Ming

    2016-01-01

    Background: Brain acid soluble protein 1 (BASP1) is identified as a novel potential tumor suppressor in several cancers. However, its role in thyroid cancer has not been investigated yet. In the present study, the antitumor activities of BASP1 against the growth and migration of thyroid cancer cells were evaluated. Methods: BASP1 expression in thyroid cancer tissues and normal tissues were examined by immunohistochemical staining and the association between its expression and prognosis was analyzed. pcDNA-BASP1 carrying full length of BASP1 cDNA was constructed to restore the expression of BASP1 in thyroid cancer cell lines (BHT-101 and KMH-2). The cell proliferation in vitro and in vivo was evaluated by WST-1 assay and xenograft tumor models, respectively. Cell cycle distribution after transfection was analyzed using flow cytometry. Cell apoptosis after transfection was examined by annexin V/propidium iodide assay. The migration was examined using transwell assay. Results: BASP1 expression was abundant in normal tissues while it is significantly decreased in cancer tissues (P = 0.000). pcDNA-BASP1 restored the expression of BASP1 and significantly inhibited the growth of BHT-101 and KMH-2 cells as well as xenograft tumors in nude mice (P = 0.000). pcDNA-BASP1 induced G1 arrest and apoptosis in BHT-101 and KMH-2 cells. In addition, pcDNA-BASP1 significantly inhibited the cell migration. Conclusions: Downregulation of BASP1 expression may play a role in the tumorigenesis of thyroid cancer. Restoration of BASP1 expression exerted extensive antitumor activities against growth and migration of thyroid cancer cells, which suggested that BASP1 gene might act as a potential therapeutic agent for the treatment of thyroid cancer. PMID:27270539

  19. Thermodynamic modelling of the effect of hydroxycarboxylic acids on the solubility of plutonium at high pH

    SciTech Connect

    Moreton, A.D.

    1993-12-31

    A number of the hydroxycarboxlyic acids generated by the alkaline degradation of cellulosic wastes under reducing conditions in a cementitious repository can significantly increase the solubility of the actinides at high pH, especially plutonium. The solubility of plutonium at pH 12, in the presence of a range of hydroxycarboxylic acids containing a number of hydroxyl groups and between one and three carboxylate groups, has been modelled using the HARPHRQ code. All the plutonium-organic complexes assumed in the model are based on a stable unit in which a central plutonium ion is bound by four oxygen atoms. The oxygen atoms can be provided either by a deprotonated hydroxyl group on one of the ligands, or by hydroxide ions.

  20. Amino acid digestibility of heat damaged distillers dried grains with solubles fed to pigs

    PubMed Central

    2013-01-01

    The primary objective of this experiment was to determine the effects of heat treatment on the standardized ileal digestibility (SID) of amino acids (AA) in corn distillers dried grains with solubles (DDGS) fed to growing pigs. The second objective was to develop regression equations that may be used to predict the concentration of SID AA in corn DDGS. A source of corn DDGS was divided into 4 batches that were either not autoclaved or autoclaved at 130°C for 10, 20, or 30 min. Four diets containing DDGS from each of the 4 batches were formulated with DDGS being the only source of AA and CP in the diets. A N-free diet also was formulated and used to determine the basal endogenous losses of CP and AA. Ten growing pigs (initial BW: 53.5 ± 3.9 kg) were surgically equipped with a T-cannula in the distal ileum and allotted to a replicated 5 × 4 Youden square design with 5 diets and 4 periods in each square. The SID of CP decreased linearly (P < 0.05) from 77.9% in non-autoclaved DDGS to 72.1, 66.1, and 68.5% in the DDGS samples that were autoclaved for 10, 20, or 30 min, respectively. The SID of lysine was quadratically reduced (P < 0.05) from 66.8% in the non-autoclaved DDGS to 54.9, 55.3, and 51.9% in the DDGS autoclaved for 10, 20, or 30 min, respectively. The concentrations of SID Arginine, Histidine, Leucine, Lysine, Methionine, Phenylalanine, or Threonine may be best predicted by equations that include the concentration of acid detergent insoluble N in the model (r2 = 0.76, 0.68, 0.67, 0.84, 0.76, 0.73, or 0.54, respectively). The concentrations of SID Isoleucine and Valine were predicted (r2 = 0.58 and 0.54, respectively) by the Lysine:CP ratio, whereas the concentration of SID Tryptophan was predicted (r2 = 0.70) by the analyzed concentration of Tryptophan in DDGS. In conclusion, the SID of AA is decreased as a result of heat damage and the concentration of SID AA in heat-damaged DDGS may be predicted by regression equations

  1. Utility of monitoring mycophenolic acid in solid organ transplant patients.

    PubMed Central

    Oremus, Mark; Zeidler, Johannes; Ensom, Mary H H; Matsuda-Abedini, Mina; Balion, Cynthia; Booker, Lynda; Archer, Carolyn; Raina, Parminder

    2008-01-01

    OBJECTIVES To investigate whether monitoring concentrations of mycophenolic acid (MPA) in the serum or plasma of persons who receive a solid organ transplant will result in a lower incidence of transplant rejections and adverse events versus no monitoring of MPA. To investigate whether the incidence of rejection or adverse events differs according to MPA dose or frequency, type of MPA, the form of MPA monitored, the method of MPA monitoring, or sample characteristics. To assess whether monitoring is cost-effective versus no monitoring. DATA SOURCES The following databases were searched from their dates of inception (in brackets) until October 2007: MEDLINE (1966); BIOSIS Previews (1976); EMBASE (1980); Cochrane Database of Systematic Reviews (1995); and Cochrane Central Register of Controlled Trials (1995). REVIEW METHODS Studies identified from the data sources went through two levels of screening (i.e., title and abstract, full text) and the ones that passed were abstracted. Criteria for abstraction included publication in the English language, study design (i.e., randomized controlled trial [RCT], observational study with comparison group, case series), and patient receipt of allograft solid organ transplant. Additionally, any form of MPA had to be measured at least once in the plasma or serum using any method of measurement (e.g., AUC0-12, C0). Furthermore, these measures had to be linked to a health outcome (e.g., transplant rejection). Certain biomarkers (e.g., serum creatinine, glomular filtration rate) and all adverse events were also considered health outcomes. RESULTS The published evidence on MPA monitoring is inconclusive. Direct, head-to-head comparison of monitoring versus no monitoring is limited to one RCT in adult, kidney transplant patients. Inferences about monitoring can be made from some observational studies, although the evidence is equivocal for MPA dose and dose frequency, nonexistent for type of MPA, inconclusive for form of MPA monitored

  2. Facile synthesis of highly efficient and recyclable magnetic solid acid from biomass waste

    PubMed Central

    Liu, Wu-Jun; Tian, Ke; Jiang, Hong; Yu, Han-Qing

    2013-01-01

    In this work, sawdust, a biomass waste, is converted into a magnetic porous carbonaceous (MPC) solid acid catalyst by an integrated fast pyrolysis–sulfonation process. The resultant magnetic solid acid has a porous structure with high surface area of 296.4 m2 g−1, which can be attributed to the catalytic effect of Fe. The catalytic activity and recyclability of the solid acid catalyst are evaluated during three typical acid-catalyzed reactions: esterification, dehydration, and hydrolysis. The favorable catalytic performance in all three reactions is attributed to the acid's high strength with 2.57 mmol g−1 of total acid sites. Moreover, the solid acid can be reused five times without a noticeable decrease in catalytic activity, indicating the stability of the porous carbon (PC)–sulfonic acid group structure. The findings in the present work offer effective alternatives for environmentally friendly utilization of abundant biomass waste. PMID:23939253

  3. Facile synthesis of highly efficient and recyclable magnetic solid acid from biomass waste.

    PubMed

    Liu, Wu-Jun; Tian, Ke; Jiang, Hong; Yu, Han-Qing

    2013-01-01

    In this work, sawdust, a biomass waste, is converted into a magnetic porous carbonaceous (MPC) solid acid catalyst by an integrated fast pyrolysis-sulfonation process. The resultant magnetic solid acid has a porous structure with high surface area of 296.4 m(2) g(-1), which can be attributed to the catalytic effect of Fe. The catalytic activity and recyclability of the solid acid catalyst are evaluated during three typical acid-catalyzed reactions: esterification, dehydration, and hydrolysis. The favorable catalytic performance in all three reactions is attributed to the acid's high strength with 2.57 mmol g(-1) of total acid sites. Moreover, the solid acid can be reused five times without a noticeable decrease in catalytic activity, indicating the stability of the porous carbon (PC)-sulfonic acid group structure. The findings in the present work offer effective alternatives for environmentally friendly utilization of abundant biomass waste. PMID:23939253

  4. Facile synthesis of highly efficient and recyclable magnetic solid acid from biomass waste

    NASA Astrophysics Data System (ADS)

    Liu, Wu-Jun; Tian, Ke; Jiang, Hong; Yu, Han-Qing

    2013-08-01

    In this work, sawdust, a biomass waste, is converted into a magnetic porous carbonaceous (MPC) solid acid catalyst by an integrated fast pyrolysis-sulfonation process. The resultant magnetic solid acid has a porous structure with high surface area of 296.4 m2 g-1, which can be attributed to the catalytic effect of Fe. The catalytic activity and recyclability of the solid acid catalyst are evaluated during three typical acid-catalyzed reactions: esterification, dehydration, and hydrolysis. The favorable catalytic performance in all three reactions is attributed to the acid's high strength with 2.57 mmol g-1 of total acid sites. Moreover, the solid acid can be reused five times without a noticeable decrease in catalytic activity, indicating the stability of the porous carbon (PC)-sulfonic acid group structure. The findings in the present work offer effective alternatives for environmentally friendly utilization of abundant biomass waste.

  5. Spectroscopic Studies of Polymer Structure in the Solid State and Water Soluble Complexes

    NASA Astrophysics Data System (ADS)

    Cha, Hyukjin

    The chemical changes before and after sulfonation of poly(ether ether ketone) (PEEK) were studied by using x-ray photoelectron spectroscopy (XPS). The inelastic mean free path (IMFP) of the photoelectrons was also measured by controlling the overlayer film thickness. The measured IMFP values for the C 1s, O 1s, S 2p and Si 2p photoelectrons were 30 +/- 3 A, 28 +/- 2 A, 34 +/- 2 Aand 35 +/- 3 A, respectively. Based on angle-resolved x-ray photoelectron spectroscopy (ARXPS) experiments, the concentration profiles and the diffusion constant D for interdiffusion of SPEEK into PEEK film could be determined. The measured diffusion coefficients varied from 3 times 10^{-15} rm cm ^2/sec (@ 583 K) to 6 times 10^{-18} (@ 443 K) cm ^2/sec. The activation energy derived from the measured diffusion coefficients was 22.8 kcal/mol. In addition, the molecular level conformational changes of poly(ether ether ketone) (PEEK) with temperature were studied by using fluorescence spectroscopy. In order to identify the origins of PEEK fluorescence, a model compound for PEEK was synthesized and characterized by UV-visible spectroscopy and fluorescence spectroscopy. The characteristic emission bands at 434 nm and 490 nm were monitored in order to understand local conformational changes of the polymer chain during the thermal treatment process. The changes in relative intensity ratio rm(I_{490}/I _{434}) were compared with differential scanning calorimeter and X-ray scattering data, and were explained in view of molecular morphology. In order to understand polymer complexation in solution, three different systems were studied. First, molecular binding between poly(acrylic acid) (PAA) and europium chloride hexahydrate rm(EuCl_3 6H_2O) and their chain conformations during the complexation process in aqueous solution was studied using fluorescence and IR spectroscopy. Second, complexation of poly(vinyl alcohol sulfate) (KPVS) with papain was investigated with fluorescence and UV absorption

  6. Solubility of Fullerenes in Fatty Acids Esters: A New Way to Deliver In Vivo Fullerenes. Theoretical Calculations and Experimental Results

    NASA Astrophysics Data System (ADS)

    Cataldo, Franco

    The biological effects of fullerenes and, in particular, of C60 have been recognized since long time. One of the problems which hindered the application of fullerenes in medicinal chemistry regards their insolubility in water and water-based fluids. In the present chapter it is reported that C60 and C70 fullerenes are soluble in vegetable oils, in general, in esters of fatty acids and in free fatty acids. These results pave the way in the utilization of vegetable oils as vehicles in the delivery of fullerenes for both topical applications and internal use (e.g., intramuscular injection).

  7. Application FT-NIR in rapid estimation of soluble solids content of intact kiwifruits by reflectance mode

    NASA Astrophysics Data System (ADS)

    Ying, Yibin; Lu, Huishan; Fu, Xiaping; Liu, Yande; Xu, Huirong; Yu, Haiyan

    2005-11-01

    Nondestructive method of measuring soluble solids content (SSC) of kiwifruit was developed by Fourier transform near infrared (FT-NIR) reflectance and fiber optics. Also, the models describing the relationship between SSC and the NIR spectra of the fruit were developed and evaluated. To develop the models several different NIR reflectance spectra were acquired for each fruit from a commercial supermarket. Different spectra correction algorithms (standard normal variate (SNV), multiplicative signal correction (MSC)) were used in this work. The relationship between laboratory SSC and FT-NIR spectra of kiwifruits were analyzed via principle component regression (PCR) and partial least squares (PLS) regression method using TQ 6.2.1 quantitative software (Thermo Nicolet Co., USA). Models based on the different spectral ranges were compared in this research. The first derivative and second derivative were applied to all measured spectra to reduce the effects of sample size, light scattering, noise of instrument, etc. Different baseline correction methods were applied to improve the spectral data quality. Among them the second derivative method after baseline correction produced best noise removing capability and to obtain optimal calibration models. Total 480 NIR spectra were acquired from 120 kiwifruits and 90 samples were used to develop the calibration model, the rest samples were used to validate the model. Developed PLS model, which describes the relationship between SSC and NIR spectra, could predict SSC of 84 unknown samples with correlation coefficient of 0.9828 and SEP of 0.679 Brix.

  8. Hyperspectral Imaging Coupled with Random Frog and Calibration Models for Assessment of Total Soluble Solids in Mulberries

    PubMed Central

    Zhao, Yan-Ru; Yu, Ke-Qiang; He, Yong

    2015-01-01

    Chemometrics methods coupled with hyperspectral imaging technology in visible and near infrared (Vis/NIR) region (380–1030 nm) were introduced to assess total soluble solids (TSS) in mulberries. Hyperspectral images of 310 mulberries were acquired by hyperspectral reflectance imaging system (512 bands) and their corresponding TSS contents were measured by a Brix meter. Random frog (RF) method was used to select important wavelengths from the full wavelengths. TSS values in mulberry fruits were predicted by partial least squares regression (PLSR) and least-square support vector machine (LS-SVM) models based on full wavelengths and the selected important wavelengths. The optimal PLSR model with 23 important wavelengths was employed to visualise the spatial distribution of TSS in tested samples, and TSS concentrations in mulberries were revealed through the TSS spatial distribution. The results declared that hyperspectral imaging is promising for determining the spatial distribution of TSS content in mulberry fruits, which provides a reference for detecting the internal quality of fruits. PMID:26451273

  9. Acute and Chronic Toxicity of Soluble Fractions of Industrial Solid Wastes on Daphnia magna and Vibrio fischeri

    PubMed Central

    Flohr, Letícia; de Castilhos Júnior, Armando Borges; Matias, William Gerson

    2012-01-01

    Industrial wastes may produce leachates that can contaminate the aquatic ecosystem. Toxicity testing in acute and chronic levels is essential to assess environmental risks from the soluble fractions of these wastes, since only chemical analysis may not be adequate to classify the hazard of an industrial waste. In this study, ten samples of solid wastes from textile, metal-mechanic, and pulp and paper industries were analyzed by acute and chronic toxicity tests with Daphnia magna and Vibrio fischeri. A metal-mechanic waste (sample MM3) induced the highest toxicity level to Daphnia magna(CE50,48 h = 2.21%). A textile waste induced the highest toxicity level to Vibrio fischeri (sample TX2, CE50,30 min = 12.08%). All samples of pulp and paper wastes, and a textile waste (sample TX2) induced chronic effects on reproduction, length, and longevity of Daphnia magna. These results could serve as an alert about the environmental risks of an inadequate waste classification method. PMID:22619632

  10. Boronic acid-containing aminopyridine- and aminopyrimidinecarboxamide CXCR1/2 antagonists: Optimization of aqueous solubility and oral bioavailability.

    PubMed

    Schuler, Aaron D; Engles, Courtney A; Maeda, Dean Y; Quinn, Mark T; Kirpotina, Liliya N; Wicomb, Winston N; Mason, S Nicholas; Auten, Richard L; Zebala, John A

    2015-09-15

    The chemokine receptors CXCR1 and CXCR2 are important pharmaceutical targets due to their key roles in inflammatory diseases and cancer progression. We have previously identified 2-[5-(4-fluoro-phenylcarbamoyl)-pyridin-2-ylsulfanylmethyl]-phenylboronic acid (SX-517) and 6-(2-boronic acid-5-trifluoromethoxy-benzylsulfanyl)-N-(4-fluoro-phenyl)-nicotinamide (SX-576) as potent non-competitive boronic acid-containing CXCR1/2 antagonists. Herein we report the synthesis and evaluation of aminopyridine and aminopyrimidine analogs of SX-517 and SX-576, identifying (2-{(benzyl)[(5-boronic acid-2-pyridyl)methyl]amino}-5-pyrimidinyl)(4-fluorophenylamino)formaldehyde as a potent chemokine antagonist with improved aqueous solubility and oral bioavailability. PMID:26248802

  11. Water-soluble organic carbon, dicarboxylic acids, ketoacids, and α-dicarbonyls in the tropical Indian aerosols

    NASA Astrophysics Data System (ADS)

    Pavuluri, Chandra Mouli; Kawamura, Kimitaka; Swaminathan, T.

    2010-06-01

    Tropical aerosol (PM10) samples (n = 49) collected from southeast coast of India were studied for water-soluble dicarboxylic acids (C2-C12), ketocarboxylic acids (C2-C9), and α-dicarbonyls (glyoxal and methylglyoxal), together with analyses of total carbon (TC) and water-soluble organic carbon (WSOC). Their distributions were characterized by a predominance of oxalic acid followed by terephthalic (t-Ph), malonic, and succinic acids. Total concentrations of diacids (227-1030 ng m-3), ketoacids (16-105 ng m-3), and dicarbonyls (4-23 ng m-3) are comparative to those from other Asian megacities such as Tokyo and Hong Kong. t-Ph acid was found as the second most abundant diacid in the Chennai aerosols. This feature has not been reported previously in atmospheric aerosols. t-Ph acid is most likely derived from the field burning of plastics. Water-soluble diacids were found to contribute 0.4%-3% of TC and 4%-11% of WSOC. Based on molecular distributions and backward air mass trajectories, we found that diacids and related compounds in coastal South Indian aerosols are influenced by South Asian and Indian Ocean monsoons. Organic aerosols are also suggested to be significantly transported long distances from North India and the Middle East in early winter and from Southeast Asia in late winter, but some originate from photochemical reactions over the Bay of Bengal. In contrast, the Arabian Sea, Indian Ocean, and South Indian continent are suggested as major source regions in summer. We also found daytime maxima of most diacids, except for C9 and t-Ph acids, which showed nighttime maxima in summer. Emissions from marine and terrestrial plants, combined with land/sea breezes and in situ photochemical oxidation, are suggested especially in summer as an important factor that controls the composition of water-soluble organic aerosols over the southeast coast of India. Regional emissions from anthropogenic sources are also important in megacity Chennai, but their influence is

  12. Pretreatment of Dried Distiller Grains with Solubles by Soaking in Aqueous Ammonia and Subsequent Enzymatic/Dilute Acid Hydrolysis to Produce Fermentable Sugars.

    PubMed

    Nghiem, Nhuan P; Montanti, Justin; Kim, Tae Hyun

    2016-05-01

    Dried distillers grains with solubles (DDGS), a co-product of corn ethanol production in the dry-grind process, was pretreated by soaking in aqueous ammonia (SAA) using a 15 % w/w NH4OH solution at a solid/liquid ratio of 1:10. The effect of pretreatment on subsequent enzymatic hydrolysis was studied at two temperatures (40 and 60 °C) and four reaction times (6, 12, 24, and 48 h). Highest glucose yield of 91 % theoretical was obtained for the DDGS pretreated at 60 °C and 24 h. The solubilized hemicellulose in the liquid fraction was further hydrolyzed with dilute H2SO4 to generate fermentable monomeric sugars. The conditions of acid hydrolysis included 1 and 4 wt% acid, 60 and 120 °C, and 0.5 and 1 h. Highest yields of xylose and arabinose were obtained at 4 wt% acid, 120 °C, and 1 h. The fermentability of the hydrolysate obtained by enzymatic hydrolysis of the SAA-pretreated DDGS was demonstrated in ethanol fermentation by Saccharomyces cerevisiae. The fermentability of the hydrolysate obtained by consecutive enzymatic and dilute acid hydrolysis was demonstrated using a succinic acid-producing microorganism, strain Escherichia coli AFP184. Under the fermentation conditions, complete utilization of glucose and arabinose was observed, whereas only 47 % of xylose was used. The succinic acid yield was 0.60 g/g total sugar consumed. PMID:26797927

  13. Proton play in the formation of low molecular weight chitosan (LWCS) by hydrolyzing chitosan with a carbon based solid acid.

    PubMed

    Krishnan, R Akhil; Deshmukh, Pranjal; Agarwal, Siddharth; Purohit, Poorvi; Dhoble, Deepa; Waske, Prashant; Khandekar, Dileep; Jain, Ratnesh; Dandekar, Prajakta

    2016-10-20

    Low molecular weight chitosan (LWCS) constitute a special class of value added chemicals that are primarily obtained from crustacean shells, which are the main water pollutants from crabs and shrimp processing centers. Unlike chitin and chitosan, LWCS possess improved solubility in water and aqueous solutions, making them widely applicable in numerous fields ranging from drug delivery to waste water treatment. Among the methods employed for their production, chemical breakdown by strong liquid acids has yielded good success. However, this method is met with severe concerns arising from the harsh nature of liquid acids, which may corrode the reactors for commercial synthesis, and their limited reusability. The physical methods like ultrasound and microwave are energy intensive in nature, while the enzymatic methods are expensive and offers limited scope for reuse. We have attempted to overcome these problems by employing carbon based solid acid (CSA) for hydrolyzing chitosan to LWCS. CSA can be easily produced using activated carbon, a cost-effective and easily available raw material. Reactions were carried out between chitosan and CSA in a hydrothermal glass reactor and the products, separated by cold centrifugation, were purified and dried. The dried products were characterized for their molecular weight and solubility. Results indicated more than ten-fold decrease in the molecular weight of chitosan and the product exhibited water solubility. The CSA could be used upto four times, without regeneration, to give a consistent quality product. The aqueous solution of resulting LWCS exhibited a pH of 6.03±0.11, as against the acidic pH range of solutions of commercially available LWCS, indicating its suitability for biomedical applications. Our investigation facilitates a 'green approach' that may be employed for commercial production of value added chemicals from waste products of marine industry. PMID:27474584

  14. Seasonal and longitudinal distributions of atmospheric water-soluble dicarboxylic acids, oxocarboxylic acids, and α-dicarbonyls over the North Pacific

    NASA Astrophysics Data System (ADS)

    Bikkina, Srinivas; Kawamura, Kimitaka; Imanishi, Katsuya; Boreddy, S. K. R.; Nojiri, Yukihiro

    2015-05-01

    In order to assess the seasonal variability of atmospheric abundances of dicarboxylic acids, oxocarboxylic acids, and α-dicarbonyls over the North Pacific and Sea of Japan, aerosol samples were collected along the longitudinal transacts during six cruises between Canada and Japan. The back trajectory analyses indicate that aerosol samples collected in winter and spring are influenced by the East Asian outflow, whereas summer and fall samples are associated with the pristine maritime air masses. Molecular distributions of water-soluble organics in winter and spring samples show the predominance of oxalic acid (C2) followed by succinic (C4) and malonic acids (C3). In contrast, summer and fall marine aerosols are characterized by the predominance of C3 over C4. Concentrations of dicarboxylic acids were higher over the Sea of Japan than the North Pacific. With a lack of continental outflow, higher concentrations during early summer are ascribed to atmospheric oxidation of organic precursors associated with high biological activity in the North Pacific. This interpretation is further supported by the high abundances of azelaic acid, which is a photochemical oxidation product of biogenic unsaturated fatty acids, over the Bering Sea in early summer when surface waters are characterized by high biological productivity. We found higher ratios of oxalic acid to pyruvic and glyoxylic acids (C2/Pyr and C2/ωC2) and glyoxal and methylglyoxal (C2/Gly and C2/MeGly) in summer and fall than in winter and spring, suggesting a production of C2 from the aqueous-phase oxidation of oceanic isoprene. In this study, dicarboxylic acids account for 0.7-38% of water-soluble organic carbon.

  15. The contribution of acidulant to the antibacterial activity of acid soluble α- and β-chitosan solutions and their films.

    PubMed

    Jung, Jooyeoun; Cavender, George; Zhao, Yanyun

    2014-01-01

    This study evaluated individual contributions of dissolving acids (acetic acid, lactic acid, and hydrochloric acid) or acid solubilized chitosan to the antibacterial activity against Listeria innocua and Escherichia coli as solutions and dried films. Solutions containing chitosan showed significantly (P < 0.05) different inhibitory activity (measured as percentage of inhibition (PI), in percent) against L. innocua and E. coli, compared to equivalent acid solutions. This increase was calculated as additional inhibition (AI, in percent), which could be as high as 65% in solutions containing 300-320 kDa chitosan depending on the acid type, bacterial species, and the chitosan form (α or β). Solutions containing 4-5 kDa chitosan had lower AI and showed much greater variability among the different chitosan forms, acid types, and bacterial species. Higher molecular weight (Mw) chitosan also showed significantly higher levels of adsorption to bacterial cells than that of lower Mw samples, suggesting that the observed increase in inhibition was the result of surface phenomena. The contribution of acids to the antibacterial activity of chitosan films was assessed by comparing non-rinsed and rinsed films (rinsed in the appropriate broth to remove residual acids and active fragments formed on the dried film). Rinsing β-chitosan films has reduced PI by as much as 28% compared with non-rinsed films, indicating that part of the antibacterial activity of chitosan films is due to the presence of soluble acid compounds and/or other active fragments. Overall, both acidulant and chitosan were found to contribute to the antibacterial activity of acid solubilized α- and β-chitosan, with the exact antibacterial activity of chitosan varying based on the solution and film properties, suggesting a complex interaction. PMID:24196584

  16. High mobility organic field-effect transistor based on water-soluble deoxyribonucleic acid via spray coating

    SciTech Connect

    Shi, Wei; Han, Shijiao; Huang, Wei; Yu, Junsheng

    2015-01-26

    High mobility organic field-effect transistors (OFETs) by inserting water-soluble deoxyribonucleic acid (DNA) buffer layer between electrodes and pentacene film through spray coating process were fabricated. Compared with the OFETs incorporated with DNA in the conventional organic solvents of ethanol and methanol: water mixture, the water-soluble DNA based OFET exhibited an over four folds enhancement of field-effect mobility from 0.035 to 0.153 cm{sup 2}/Vs. By characterizing the surface morphology and the crystalline structure of pentacene active layer through atomic force microscope and X-ray diffraction, it was found that the adoption of water solvent in DNA solution, which played a key role in enhancing the field-effect mobility, was ascribed to both the elimination of the irreversible organic solvent-induced bulk-like phase transition of pentacene film and the diminution of a majority of charge trapping at interfaces in OFETs.

  17. Enhancing the intestinal absorption of poorly water-soluble weak-acidic compound by controlling local pH.

    PubMed

    Iwanaga, Kazunori; Kato, Shino; Miyazaki, Makoto; Kakemi, Masawo

    2013-12-01

    Recently, the number of poorly water-soluble drug candidates has increased and has hindered the rapid improvement of new drugs with low intestinal absorption; however, the intestinal absorption of pH-dependent poorly water-soluble compounds is expected to be markedly improved by changing the pH in the vicinity of the absorption site. The aim of this study is to clarify the effect of local pH change in the intestinal tract by magnesium oxide on the intestinal absorption of hydrochlorothiazide, a model poorly water-soluble weak-acid compound. The application of hydrochlorothiazide granule containing magnesium oxide to the rat intestinal loop increased the pH in the vicinity of the dosing site to more than 8.5 for 90 min without any mucosal damage. As a result, absorption of hydrochlorothiazide increased by the addition of magnesium oxide to the granule. Intraintestinal administration of a suspension prepared from hydrochlorothiazide granules with magnesium oxide increased the intestinal absorption and the AUC value was 3-fold higher than that without magnesium oxide. To further increase the intestinal absorption of hydrochlorothiazide, we prepared granules containing magnesium oxide and chitosan as a mucoadhesive and tight junction opening material. Chitosan showed a marked increase of intestinal absorption, and the AUC value after the administration of suspensions of chitosan granules was more than 5-fold higher than that of granules containing hydrochlorothiazide alone, respectively. In summary, it has been clarified that the intestinal absorption of weak-acidic poorly water-soluble compound can be enhanced by increasing local pH, mucoadhesion and opening tight junction. PMID:22443480

  18. [Determination of soluble solids content in Nanfeng Mandarin by Vis/NIR spectroscopy and UVE-ICA-LS-SVM].

    PubMed

    Sun, Tong; Xu, Wen-Li; Hu, Tian; Liu, Mu-Hua

    2013-12-01

    The objective of the present research was to assess soluble solids content (SSC) of Nanfeng mandarin by visible/near infrared (Vis/NIR) spectroscopy combined with new variable selection method, simplify prediction model and improve the performance of prediction model for SSC of Nanfeng mandarin. A total of 300 Nanfeng mandarin samples were used, the numbers of Nanfeng mandarin samples in calibration, validation and prediction sets were 150, 75 and 75, respectively. Vis/NIR spectra of Nanfeng mandarin samples were acquired by a QualitySpec spectrometer in the wavelength range of 350-1000 nm. Uninformative variables elimination (UVE) was used to eliminate wavelength variables that had few information of SSC, then independent component analysis (ICA) was used to extract independent components (ICs) from spectra that eliminated uninformative wavelength variables. At last, least squares support vector machine (LS-SVM) was used to develop calibration models for SSC of Nanfeng mandarin using extracted ICs, and 75 prediction samples that had not been used for model development were used to evaluate the performance of SSC model of Nanfeng mandarin. The results indicate t hat Vis/NIR spectroscopy combinedwith UVE-ICA-LS-SVM is suitable for assessing SSC o f Nanfeng mandarin, and t he precision o f prediction ishigh. UVE--ICA is an effective method to eliminate uninformative wavelength variables, extract important spectral information, simplify prediction model and improve the performance of prediction model. The SSC model developed by UVE-ICA-LS-SVM is superior to that developed by PLS, PCA-LS-SVM or ICA-LS-SVM, and the coefficient of determination and root mean square error in calibration, validation and prediction sets were 0.978, 0.230%, 0.965, 0.301% and 0.967, 0.292%, respectively. PMID:24611377

  19. Ultraviolet-visible transmittance techniques for rapid analysis of sugar content and soluble solids content of fresh navel orange juices

    NASA Astrophysics Data System (ADS)

    Liu, Yande; Ouyang, Aiguo; Luo, Ji; Ying, Yibin

    2005-11-01

    Sugar content (SC) and soluble solids content (SSC) are very important factors of navel orange internal quality and can be measured non-invasively by ultraviolet-visible spectroscopy techniques. The feasibility and methods of ultraviolet-visible spectroscopic techniques for rapid quantifying SC and SSC of navel orange fresh juices was investigated by its spectral transmittance. A total 55 juice samples were used to develop the calibration and prediction models. Different spectra correction algorithms (constant, multiplicative signal correction (MSC) and standard normal variate (SNV) were compared in our work. Three different kinds of mathematical spectra treatments (original, first derivative and second derivative) of spectra in the range of 200-800 nm and two kinds of reference standards were also investigated. Three kinds of models including partial least square regression (PLSR), stepwise multiple linear regression (SMLR) and principle component regression (PCR) were evaluated for the determination of SC and SSC in navel orange juice. Calibration models based on the different spectral ranges were also compared. Performance of different models was assessed in terms of root mean square errors of prediction (RMSEP) and correlation coefficient (r) of prediction set of samples. The correlation coefficients of calibration models for SC and SSC were 0.965 and 0.961, the correlation coefficients of prediction models for SC and SSC were 0.857 and 0.888, and the corresponding RMSEP were 0.562 and 0.492 respectively. The results show that ultraviolet-visible transmittance technique is a feasible method for non-invasive estimation of fruit juice SC and SSC.

  20. Polymorphism in sulfadimidine/4-aminosalicylic acid cocrystals: solid-state characterization and physicochemical properties.

    PubMed

    Grossjohann, Christine; Serrano, Dolores R; Paluch, Krzysztof J; O'Connell, Peter; Vella-Zarb, Liana; Manesiotis, Panagiotis; Mccabe, Thomas; Tajber, Lidia; Corrigan, Owen I; Healy, Anne Marie

    2015-04-01

    Polymorphism of crystalline drugs is a common phenomenon. However, the number of reported polymorphic cocrystals is very limited. In this work, the synthesis and solid-state characterization of a polymorphic cocrystal composed of sulfadimidine (SD) and 4-aminosalicylic acid (4-ASA) is reported for the first time. By liquid-assisted milling, the SD:4-ASA 1:1 form I cocrystal, the structure of which has been previously reported, was formed. By spray drying, a new polymorphic form (form II) of the SD:4-ASA 1:1 cocrystal was discovered which could also be obtained by solvent evaporation from ethanol and acetone. Structure determination of the form II cocrystal was calculated using high-resolution X-ray powder diffraction. The solubility of the SD:4-ASA 1:1 cocrystal was dependent on the pH and predicted by a model established for a two amphoteric component cocrystal. The form I cocrystal was found to be thermodynamically more stable in aqueous solution than form II, which showed transformation to form I. Dissolution studies revealed that the dissolution rate of SD from both cocrystals was enhanced when compared with a physical equimolar mixture and pure SD. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association J Pharm Sci 104:1385-1398, 2015. PMID:25605031

  1. Assessment of hupu gum for its carrier property in the design and evaluation of solid mixtures of poorly water soluble drug - rofecoxib.

    PubMed

    Vadlamudi, Harini Chowdary; Raju, Y Prasanna; Asuntha, G; Nair, Rahul; Murthy, K V Ramana; Vulava, Jayasri

    2014-01-01

    There are no reports about the pharmaceutical applications of hupu gum (HG). Hence the present study was undertaken to test its suitability in the dissolution enhancement of poorly water soluble drug. Rofecoxib (RFB) was taken as model drug. For comparison solid mixtures were prepared with carriers such as poly vinyl pyrrolidone (PVP), sodium starch glycollate (SSG) and guar gum (GG). Physical mixing (PM), co-grinding (CG), kneading (KT) and solvent evaporation (SE) techniques were used to prepare the solid mixtures, using all the carriers in different carrier and drug ratios. The solid mixtures were characterized by powder X-ray diffraction (XRD) and Fourier-transformed infrared spectroscopy (FTIR). There was a significant improvement in the dissolution rate of solid mixtures of HG, when compared with the solid mixtures of other carriers. There was an increase in dissolution rate with increase in concentration of HG upto 1:1 ratio of carrier and drug. No drug-carrier interaction was found by FTIR studies. XRD studies indicated reduction in crystallinity of the drug with increase in HG concentration. Hence HG could be a useful carrier for the dissolution enhancement of poorly water soluble drugs. PMID:24783235

  2. Water-soluble dicarboxylic acids and ω-oxocarboxylic acids in size-segregated aerosols over northern Japan during spring: sources and formation processes

    NASA Astrophysics Data System (ADS)

    Deshmukh, Dhananjay Kumar; Kawamura, Kimitaka; Kobayashi, Minoru; Gowda, Divyavani

    2016-04-01

    Seven sets (AF01-AF07) of size-segregated aerosol (12-sizes) samples were collected using a Micro-Orifice Uniform Deposit Impactor (MOUDI) in Sapporo, Japan during the spring of 2001 to understand the sources and atmospheric processes of water-soluble organic aerosols in the outflow region of Asian dusts. The samples were analyzed for dicarboxylic acids (C2-C12) and ω-oxocarboxylic acids as well as inorganic ions. The molecular distribution of diacids showed the predominance of oxalic acid (C2) followed by malonic and succinic acids whereas ω-oxoacids showed the predominance of glyoxylic acid (ωC2) in size-segregated aerosols. SO42- and NH4+ are enriched in submicron mode whereas NO3- and Ca2+ are in supermicron mode. Most of diacids and ω-oxoacids are enriched in supermicron mode in the samples (AF01-AF03) influenced by the long-range transport of mineral dusts whereas enhanced presence in submicron mode was observed in other sample sets. The strong correlations of C2 with Ca2+ (r = 0.95-0.99) and NO3- (r = 0.96-0.98) in supermicron mode in the samples AF01-AF03 suggest the adsorption or production of C2 diacid via heterogeneous reaction on the surface of mineral dust during long-range atmospheric transport. The preferential enrichment of diacids and ω-oxoacids in mineral dust has important implications for the solubility and cloud nucleation properties of the dominant fraction of water-soluble organic aerosols. This study demonstrates that biofuel and biomass burning and mineral dust originated in East Asia are two major factors to control the size distribution of diacids and related compounds over northern Japan.

  3. Synthesis, characterization, solubility and stability studies of hydrate cocrystal of antitubercular Isoniazid with antioxidant and anti-bacterial Protocatechuic acid

    NASA Astrophysics Data System (ADS)

    Mashhadi, Syed Muddassir Ali; Yunus, Uzma; Bhatti, Moazzam Hussain; Ahmed, Imtiaz; Tahir, Muhammad Nawaz

    2016-08-01

    Isoniazid is an important component used in "triple therapy" to combat tuberculosis. It has reduced Tabletting formulations stability. Anti-oxidants are obligatory to counter oxidative stress, pulmonary inflammation, and free radical burst from macrophages caused in tuberculosis and other diseases. In the present study a hydrate cocrystal of Isoniazid with anti-oxidant and anti-inflammatory and anti-bacterial Protocatechuic acid (3,4-dihydroxybenzoic acid) in 1:1 is reported. This Cocrystal may have improved tabletting stability and anti-oxidant properties. Cocrystal structure analysis confirmed the existence of pyridine-carboxylic acid synthon in the Cocrystal. Other synthons of different graph sets involving Nsbnd H···O and Osbnd H···N bonds are formed between hydrazide group of isoniazid and coformer. Solubility studies revealed that cocrystal is less soluble as compared to isoniazid in buffer at pH 7.4 at 22 °C while stability studies at 80 °C for 24 h period disclosed the fact that cocrystal has higher stability than that of isoniazid.

  4. Transcripts for genes encoding soluble acid invertase and sucrose synthase accumulate in root tip and cortical cells containing mycorrhizal arbuscules.

    PubMed

    Blee, Kristopher A; Anderson, Anne J

    2002-09-01

    Arbuscule formation by the arbuscular mycorrhizal fungus Glomus intraradices (Schenck & Smith) was limited to cortical cells immediately adjacent to the endodermis. Because these cortical cells are the first to intercept photosynthate exiting the vascular cylinder, transcript levels for sucrose metabolizing-enzymes were compared between mycorrhizal and non-mycorrhizal roots. The probes corresponded to genes encoding a soluble acid invertase with potential vacuolar targeting, which we generated from Phaseolus vulgaris roots, a Rhizobium-responsive sucrose synthase of soybean and a cell wall acid invertase of carrot. Transcripts in non-mycorrhizal roots were developmentally regulated and abundant in the root tips for all three probes but in differentiated roots of P. vulgaris they were predominantly located in phloem tissues for sucrose synthase or the endodermis and phloem for soluble acid invertase. In mycorrhizal roots increased accumulations of transcripts for sucrose synthase and vacuolar invertase were both observed in the same cortical cells bearing arbuscules that fluoresce. There was no effect on the expression of the cell wall invertase gene in fluorescent carrot cells containing arbuscules. Thus, it appears that presence of the fungal hyphae in the fluorescent arbusculated cell stimulates discrete alterations in expression of sucrose metabolizing enzymes to increase the sink potential of the cell. PMID:12175013

  5. A comparison of water solubility enhancements of organic solutes by aquatic humic materials and commercial humic acids

    USGS Publications Warehouse

    Chlou, C.T.; Kile, D.E.; Brinton, T.I.; Malcolm, R.L.; Leenheer, J.A.; MacCarthy, P.

    1987-01-01

    Water solubility enhancements of 1,1-bis(p-chloro-phenyl)-2,2,2-trichloroethane (p,p???-DDT), 2,4,5,2???,5???-pentachlorobiphenyl (2,4,5,2???,5???-PCB), and 2,4,4???-tri-chlorobiphenyl (2,4,4???-PCB) by dissolved organic matter have been studied with the following samples: (1) acidic water samples from the Suwannee River, Georgia, and the Sopchoppy River, Florida; (2) a humic extract of a nearly neutral pH water from the Calcasieu River, Louisiana; (3) commercial humic acids from the Aldrich Chemical Co. and Fluka-Tridom Chemical Corp. The calculated partition coefficients on a dissolved organic carbon basis (Kdoc) for organic solutes with water samples and aquatic humic extracts from this and earlier studies indicate that the enhancement effect varies with the molecular composition of the aquatic humic materials. The Kdoc values with water and aquatic humic samples are, however, far less than the observed Kdoc values obtained with the two commercial samples, by factors of about 4-20. In view of this finding, one should be cautious in interpreting the effects of the dissolved organic matter on solubility enhancement of organic solutes on the basis of the use of commercial humic acids.

  6. The Changes in Color, Soluble Sugars, Organic Acids, Anthocyanins and Aroma Components in "Starkrimson" during the Ripening Period in China.

    PubMed

    Liu, Yulian; Chen, Nianlai; Ma, Zonghuan; Che, Fei; Mao, Juan; Chen, Baihong

    2016-01-01

    "Starkrimson" is a traditional apple cultivar that was developed a long time ago and was widely cultivated in the arid region of the northern Wei River of China. However, little information regarding the quality characteristics of "Starkrimson" fruit has been reported in this area. To elucidate these characteristics, the color, soluble sugars, organic acids, anthocyanins and aroma components were measured during the ripening period through the use of high performance liquid chromatography (HPLC) and gas chromatography-mass spectrometry (GC-MS). The results indicated that the changes in anthocyanin contents took place later than the changes in the Commission International Eclairage (CIE) parameters. Meanwhile, cyanidin 3-galactoside (cy3-gal), fructose, sucrose, glucose and malic acid were the primary organic compounds, and 1-butanol-2-methyl-acetate, 2-hexenal and 1-hexanol were the most abundant aroma components in the skin. Furthermore, rapidly changing soluble sugars and organic acid synchronization took place in the early ripening period, while rapidly changing aroma components occurred later, on the basis of fresh weight. This result suggested that the production of aroma components might be a useful index of apple maturity. PMID:27338331

  7. Thermal inactivation of Alicyclobacillus acidoterrestris spores under different temperature, soluble solids and pH conditions for the design of fruit processes.

    PubMed

    Silva, F M; Gibbs, P; Vieira, M C; Silva, C L

    1999-10-15

    Alicyclobacillus acidoterrestris, a thermoacidophilic, non-pathogenic and spore-forming bacterium has been detected in several spoiled commercial pasteurised fruit juices. A. acidoterrestris spores, besides being resistant to the pasteurisation treatment conditions normally applied to acidic fruit products, can germinate and grow causing spoilage. Therefore, this microorganism was suggested as the target to be used in the design of adequate pasteurisation processes. The objectives of this work were to investigate the influence of temperature (T: 85-97 degrees C), total soluble solids (SS: 5-60 degrees Brix or % by weight) and pH (2.5-6.0) on D-values (decimal reduction time) of Alicyclobacillus acidoterrestris (type strain, NCIMB 13137) spores, and to fit a model using response surface methodology. A central composite face-centred experimental design was used, and the response, D-value determined in malt extract broth, ranged between 0.498+/-0.045 and 94.9+/-6.7 min. Within the factor ranges studied, temperature was the parameter that most affected the D-value. Following this was the SS and, lastly, the pH value. A linear decrease in D-value was observed with decreasing SS and pH, and a non-linear decrease in D-value was noticed with increasing temperature. A second order polynomial was successfully fitted to the data (R2 = 0.98). In general, D-values measured in real fruit systems, such as orange, apple and grape juices, blackcurrant concentrates, cupuaçu (exotic fruit) extract and orange juice drink, were higher than those predicted by the malt extract broth model. This result emphasises the importance of experimental validation of any model-derived process. PMID:10574085

  8. Molecular weight distribution of soluble fiber fractions and short chain fatty acids in ileal digesta of growing pigs.

    PubMed

    Ivarsson, E; Andersson, R; Lindberg, J E

    2012-12-01

    The effect of dietary fiber source on molecular weight (MW) distribution of soluble fiber fractions and short chain fatty acids (SCFA) in ileal digesta of 7 post valve T-cecum (PVTC) cannulated growing pigs was studied. Pigs were fed semisynthetic diets with sugar beet (Beta vulgaris) pulp (SBP) or chicory (Cichorium intybus) forage (CFO) as fiber sources of which the soluble nonstarch polysaccharide (NSP) fraction originated mainly from pectin. Three MW intervals were selected-large MW (MWL): 10,000,000 to 1,000,000 g/mol, medium MW (MWM): 1,000,000 to 200,000 g/mol, and small MW (MWS): 200,000 to 10,000 g/mol-and the relative distribution (% of total) of molecules in each interval was calculated. The MWM fraction was higher (P < 0.05) in ileal digesta of pigs fed diet SBP and the MWS fraction was higher (P < 0.05) in ileal digesta of pigs fed diet CFO. The mole/100 mole of propionic acid (HPr) was higher (P < 0.010) in pigs fed diet SBP whereas pigs fed diet CFO had higher (P < 0.010) mole/100 mole of acetic acid (HAc). The proportion of the MWL and MWM fractions in ileal digesta were negatively correlated to HAc (r = -0.52, P = 0.05, and r = -0.62, P = 0.02, respectively). The proportion of MWM in ileal digesta was positively correlated to HPr (r = 0.83; P = 0.001) whereas MWS and HPr were negatively correlated (r = -0.76; P = 0.002). In conclusion, the bacterial degradation of the soluble NSP fraction is selective and MW distribution may explain differences in SCFA production. PMID:23365284

  9. Effect of Different Inclusion Level of Condensed Distillers Solubles Ratios and Oil Content on Amino Acid Digestibility of Corn Distillers Dried Grains with Solubles in Growing Pigs

    PubMed Central

    Li, P.; Xu, X.; Zhang, Q.; Liu, J. D.; Li, Q. Y.; Zhang, S.; Ma, X. K.; Piao, X. S.

    2015-01-01

    The purpose of this experiment was to determine and compare the digestibility of crude protein (CP) and amino acids (AA) in full-oil (no oil extracted) and de-oiled (oil extracted) corn distillers dried grains with solubles (DDGS) with different condensed distillers solubles (CDS) ratios. Six barrows (29.6±2.3 kg) fitted with ileal T-cannula were allotted into a 6×6 Latin square design. Each period was comprised of a 5-d adaption period followed by a 2-d collection of ileal digesta. The five test diets contained 62% DDGS as the sole source of AA. A nitrogen-free diet was used to measure the basal endogenous losses of CP and AA. Chromic oxide (0.3%) was used as an index in each diet. The results showed that CP and AA were very similar in 5 DDGS, but the standardized ileal digestibility (SID) of lysine (from 56.16% to 71.15%) and tryptophan (from 54.90% to 68.38%) had the lowest values and largest variation within the essential AA, which suggests reduced availability of AA and different levels of Maillard reactions in the five DDGS. The apparent ileal digestibility and SID of CP and most of AA in full-oil DDGS (sources 1 and 2) were greater (p<0.05) than de-oiled DDGS (sources 3, 4, and 5). Comparing the AA SID in the 5 DDGS, full-oil with low CDS ratio DDGS (source 1) had non-significantly higher values (p >0.05) than full-oil with high CDS ratio DDGS (source 2); however, the SID of most AA of de-oiled with low CDS ratios DDGS (source 3) were non-significantly lower (p>0.05) than de-oiled with high CDS ratio DDGS (source 4); and the de-oiled DDGS with middle CDS ratio (source 5) but with different drying processing had the lowest SID AA values. In conclusion, de-oiled DDGS had lower SID of CP and AA than full-oil DDGS; a higher CDS ratio tended to decrease the SID of AA in full-oil DDGS but not in de-oiled DDGS; and compared with CDS ratio, processing, especially drying, may have more of an effect on AA digestibility of DDGS. PMID:25557681

  10. Binding and solubility of oleic acid to laboratory materials: A possible artifact

    SciTech Connect

    Mailman, D.; Rose, C. )

    1990-01-01

    The possibility that significant amounts of fatty acids were dissolved in or bound to the surfaces of common laboratory materials was examined. The uptake or adsorption of radioisotopically labeled oleic acid and cholic acid by plastic tubing of Tygon{trademark}, Teflon{trademark}, and polyethylene, and Pyrex{trademark}, and borosilicate glass, and steel was measured. {sup 3}H-oleic acid and {sup 14}C-cholic acid were used in the presence of different concentration of unlabeled oleic acid, cholic acid, and/or bovine serum albumin. Concentrations, composition, pH, and perfusion rates were varied. Relatively large amounts of oleic acid were lost by dissolving in plastic and adsorption to glass or metal. The degree of losses decreased in the presence of compounds in the perfusion solution which could bind or dissolve oleic acid. In contrast, cholic acid was not lost to plastic, glass or metal. The magnitude of and influence of perfusion rate, composition, pH, and sequence of perfusion solutions on oleic acid losses were sufficiently large that the results of certain studies, such as those of unstirred water layers or albumin-stimulated fatty acid uptake by hepatocytes may need to be reexamined.

  11. The relationship between surface tension and the industrial performance of water-soluble polymers prepared from acid hydrolysis lignin, a saccharification by-product from woody materials.

    PubMed

    Matsushita, Yasuyuki; Imai, Masanori; Iwatsuki, Ayuko; Fukushima, Kazuhiko

    2008-05-01

    In this study, water-soluble anionic and cationic polymers were prepared from sulfuric acid lignin (SAL), an acid hydrolysis lignin, and the relationship between the surface tension of these polymers and industrial performance was examined. The SAL was phenolized (P-SAL) to enhance its solubility and reactivity. Sulfonation and the Mannich reaction with aminocarboxylic acids produced water-soluble anionic polymers and high-dispersibility gypsum paste. The dispersing efficiency increased as the surface tension decreased, suggesting that the fluidity of the gypsum paste increased with the polymer adsorption on the gypsum particle surface. Water-soluble cationic polymers were prepared using the Mannich reaction with dimethylamine. The cationic polymers showed high sizing efficiency under neutral papermaking conditions; the sizing efficiency increased with the surface tension. This suggests that the polymer with high hydrophilicity spread in the water and readily adhered to the pulp surface and the rosin, showing good retention. PMID:17664066

  12. Uptake of acid pollutants by mineral dust and their effect on aerosol solubility

    NASA Astrophysics Data System (ADS)

    Saliba, N. A.; Chamseddine, Ashraf

    2012-01-01

    Due to the implications caused by mineral dust and sea-salt heterogeneous reactions with SO 2, NO x and NH 3 derivatives, this study aims to understand the interaction between gaseous and particulate phases; PM10 and PM2.5, in dust-rich and dust-poor environments. During dust outbreaks, the increase in PM10 and PM2.5 mass concentrations by 80 and 75%, respectively, was accompanied with approximately 30% decrease in water soluble inorganic ions. However, nitrate ion concentration, which increased by 36% during dust-rich episodes, was correlated with a 96% increase in gaseous HONO concentration. This implies a significant impact of dust storms on the tropospheric NO 2 to HONO conversion and consequently the formation of nitrate in PMs. Products of the reaction between HONO and mineral dust render atmospheric aerosols more soluble and consequently higher nitrogen deposition fluxes were calculated.

  13. Esterification of pseudoephedrine hydrochloride by citric acid in a solid dose pharmaceutical preparation.

    PubMed

    Goel, Alok; Zhao, Zhicheng; Sørensen, Dan; Zhou, Jay; Zhang, Fa

    2016-09-10

    Esterification of pseudoephedrine hydrochloride (PSE) by citric acid was observed in a solid dose pharmaceutical preparation at room temperature and accelerated stability condition (40°C/75% relative humidity). The esterification of PSE with citric acid was confirmed by a solid-state binary reaction in the presence of minor level of water at elevated temperature to generate three isomeric esters. The structures of the pseudoephedrine citric acid esters were elucidated using high-resolution mass spectrometry and nuclear magnetic resonance spectroscopy (NMR). Occurrence of esterification in solid state, instead of amidation which is generally more favorable than esterification, is likely due to remaining HCl salt form of solid pseudoephedrine hydrochloride to protect its amino group from amidation with citric acid. In contrast, the esterification was not observed from solution reaction between PSE and citric acid. PMID:27474946

  14. High abundances of water-soluble dicarboxylic acids, ketocarboxylic acids and α-dicarbonyls in the mountaintop aerosols over the North China Plain during wheat burning season

    NASA Astrophysics Data System (ADS)

    Kawamura, K.; Tachibana, E.; Okuzawa, K.; Aggarwal, S. G.; Kanaya, Y.; Wang, Z. F.

    2013-08-01

    Aerosol (TSP) samples were collected at the summit of Mount Tai (elevation: 1534 m a.s.l., 36.25° N, 117.10° E) located in the North China Plain using a high-volume air sampler and pre-combusted quartz filters. Sampling was conducted on day/night or 3 h basis in the period from 29 May to 28 June 2006 during the field burning of wheat straw residue and the post-burning season. The filter samples were analyzed for low-molecular-weight dicarboxylic acids, ketoacids and α-dicarbonyls using capillary gas chromatography (GC) and GC-MS employing water extraction and butyl ester derivatization. Molecular distributions of dicarboxylic acids (C2-C11, 220-6070 ng m-3) were characterized by a predominance of oxalic (C2) acid (105-3920 ng m-3) followed by succinic (C4) or malonic (C3) acid. Unsaturated aliphatic diacids, including maleic (M), isomaleic (iM) and fumaric (F) acids, were also detected together with aromatic diacids (phthalic, isophthalic and terephthalic acids). ω-oxocarboxylic acids (C2-C9, 24-610 ng m-3) were detected as the second most abundant compound class with the predominance of glyoxylic acid (11-360 ng m-3), followed by α-ketoacid (pyruvic acid, 3-140 ng m-3) and α-dicarbonyls (glyoxal, 1-230 ng m-3 and methylglyoxal, 2-120 ng m-3). We found that these levels (>6000 ng m-3 for diacids) are several times higher than those reported in Chinese megacities at ground levels. The concentrations of diacids increased from late May to early June, showing a maximum on 7 June, and then significantly decreased during the period 8-11 June, when the wind direction shifted from southerly to northerly. Similar temporal trends were found for ketocarboxylic acids and α-dicarbonyls as well as total carbon (TC) and water-soluble organic carbon (WSOC). The temporal variations of water-soluble organics were interpreted by the direct emission from the field burning of agricultural wastes (wheat straw) in the North China Plain and the subsequent photochemical oxidation of

  15. In vitro oxidation of indoleacetic acid by soluble auxin-oxidases and peroxidases from maize roots. [Zea mays L

    SciTech Connect

    Beffa, R.; Martin, H.V.; Pilet, P.E. )

    1990-10-01

    Soluble auxin-oxidases were extracted from Zea mays L. cv LG11 apical root segments and partially separated from peroxidases (EC 1.11.1.7) by size-exclusion chromatography. Auxin-oxidases were resolved into one main peak corresponding to a molecular mass of 32.5 kilodaltons and a minor peak at 54.5 kilodaltons. Peroxidases were separated into at least four peaks, with molecular masses from 32.5 to 78 kilodaltons. In vitro activity of indoleacetic acid-oxidases was dependent on the presence of MnCl{sub 2} and p-coumaric acid. Compound(s) present in the crude extract and several synthetic auxin transport inhibitors (including 2,3,5-triiodobenzoic acid and N-1-naphthylphthalamic acid) inhibited auxin-oxidase activity, but had no effect on peroxidases. The products resulting from the in vitro enzymatic oxidation of ({sup 3}H)indoleacetic acid were separated by HPLC and the major metabolite was found to cochromatograph with indol-3yl-methanol.

  16. Protection from hypertension in mice by the Mediterranean diet is mediated by nitro fatty acid inhibition of soluble epoxide hydrolase

    PubMed Central

    Charles, Rebecca L.; Rudyk, Olena; Prysyazhna, Oleksandra; Kamynina, Alisa; Yang, Jun; Morisseau, Christophe; Hammock, Bruce D.; Freeman, Bruce A.; Eaton, Philip

    2014-01-01

    Soluble epoxide hydrolase (sEH) is inhibited by electrophilic lipids by their adduction to Cys521 proximal to its catalytic center. This inhibition prevents hydrolysis of the enzymes’ epoxyeicosatrienoic acid (EET) substrates, so they accumulate inducing vasodilation to lower blood pressure (BP). We generated a Cys521Ser sEH redox-dead knockin (KI) mouse model that was resistant to this mode of inhibition. The electrophilic lipid 10-nitro-oleic acid (NO2-OA) inhibited hydrolase activity and also lowered BP in an angiotensin II-induced hypertension model in wild-type (WT) but not KI mice. Furthermore, EET/dihydroxy-epoxyeicosatrienoic acid isomer ratios were elevated in plasma from WT but not KI mice following NO2-OA treatment, consistent with the redox-dead mutant being resistant to inhibition by lipid electrophiles. sEH was inhibited in WT mice fed linoleic acid and nitrite, key constituents of the Mediterranean diet that elevates electrophilic nitro fatty acid levels, whereas KIs were unaffected. These observations reveal that lipid electrophiles such as NO2-OA mediate antihypertensive signaling actions by inhibiting sEH and suggest a mechanism accounting for protection from hypertension afforded by the Mediterranean diet. PMID:24843165

  17. Increase on the Initial Soluble Heme Levels in Acidic Conditions Is an Important Mechanism for Spontaneous Heme Crystallization In Vitro

    PubMed Central

    Egan, Timothy J.; Wright, David W.; Oliveira, Marcus F.

    2010-01-01

    Background Hemozoin (Hz) is a heme crystal that represents a vital pathway for heme disposal in several blood-feeding organisms. Recent evidence demonstrated that β-hematin (βH) (the synthetic counterpart of Hz) formation occurs under physiological conditions near synthetic or biological hydrophilic-hydrophobic interfaces. This seems to require a heme dimer acting as a precursor of Hz crystals that would be formed spontaneously in the absence of the competing water molecules bound to the heme iron. Here, we aimed to investigate the role of medium polarity on spontaneous βH formation in vitro. Methodology/Principal Findings We assessed the effect of water content on spontaneous βH formation by using the aprotic solvent dimethylsulfoxide (DMSO) and a series of polyethyleneglycols (PEGs). We observed that both DMSO and PEGs (3.350, 6.000, 8.000, and 22.000) increased the levels of soluble heme under acidic conditions. These compounds were able to stimulate the production of βH crystals in the absence of any biological sample. Interestingly, the effects of DMSO and PEGs on βH formation were positively correlated with their capacity to promote previous heme solubilization in acidic conditions. Curiously, a short chain polyethyleneglycol (PEG 300) caused a significant reduction in both soluble heme levels and βH formation. Finally, both heme solubilization and βH formation strongly correlated with reduced medium water activity provided by increased DMSO concentrations. Conclusions The data presented here support the notion that reduction of the water activity is an important mechanism to support spontaneous heme crystallization, which depends on the previous increase of soluble heme levels. PMID:20856937

  18. Utilization of Condensed Distillers Solubles as Nutrient Supplement for Production of Nisin and Lactic Acid from Whey

    NASA Astrophysics Data System (ADS)

    Liu, Chuanbin; Hu, Bo; Chen, Shulin; Glass, Richard W.

    The major challenge associated with the rapid growth of the ethanol industry is the usage of the coproducts, i.e., condensed distillers solubles (CDS) and distillers dried grains, which are currently sold as animal feed supplements. As the growth of the livestock industries remains flat, alternative usage of these coproducts is urgently needed. CDS is obtained after the removal of ethanol by distillation from the yeast fermentation of a grain or a grain mixture by condensing the thin stillage fraction to semisolid. In this work, CDS was first characterized and yeast biomass was proven to be the major component of CDS. CDS contained 7.50% crude protein but with only 42% of that protein being water soluble. Then, CDS was applied as a nutrient supplement for simultaneous production of nisin and lactic acid by Lactococcus lactis subsp. lactis (ATCC 11454). Although CDS was able to support bacteria growth and nisin production, a strong inhibition was observed when CDS was overdosed. This may be caused by the existence of the major ethanol fermentation byproducts, especially lactate and acetate, in CDS. In the final step, the CDS based medium composition for nisin and lactic acid production was optimized using response surface methodology.

  19. Solubility and crystallographic facet tailoring of (GaN)1-x(ZnO)x pseudobinary solid-solution nanostructures as promising photocatalysts

    NASA Astrophysics Data System (ADS)

    Li, Jing; Liu, Baodan; Yang, Wenjin; Cho, Yujin; Zhang, Xinglai; Dierre, Benjamin; Sekiguchi, Takashi; Wu, Aimin; Jiang, Xin

    2016-02-01

    (GaN)1-x(ZnO)x solid-solution nanostructures with superior crystallinity, large surface areas and visible light absorption have been regarded as promising photocatalysts for overall water splitting to produce H2. In this work, we report the preparation of (GaN)1-x(ZnO)x solid-solution nanorods with a high ZnO solubility up to 95% via a two-step synthetic route, which starts from a sol-gel reaction and follows with a nitridation process. Moreover, we clearly demonstrated that the crystallographic facets of (GaN)1-x(ZnO)x solid-solution nanorods can be finely tailored from non-polar {101&cmb.macr;0} to semipolar {101&cmb.macr;1} and then finally to mixed {101&cmb.macr;1} and polar {0001&cmb.macr;} by carefully controlling the growth temperature and nitridation time. Correspondingly, the ZnO content in the GaN lattice can be achieved in the range of ~25%-95%. Room-temperature cathodoluminescence (CL) measurements on the three types of (GaN)1-x(ZnO)x solid-solution nanorods indicate that the minimum band-gap of 2.46 eV of the solid-solution nanorods is achieved under a ZnO solubility of 25%. The efficiency and versatility of our strategy in the band-gap and facet engineering of (GaN)1-x(ZnO)x solid-solution nanorods will enhance their promising photocatalytic utilizations like an overall water splitting for H2 production under visible-light irradiation.(GaN)1-x(ZnO)x solid-solution nanostructures with superior crystallinity, large surface areas and visible light absorption have been regarded as promising photocatalysts for overall water splitting to produce H2. In this work, we report the preparation of (GaN)1-x(ZnO)x solid-solution nanorods with a high ZnO solubility up to 95% via a two-step synthetic route, which starts from a sol-gel reaction and follows with a nitridation process. Moreover, we clearly demonstrated that the crystallographic facets of (GaN)1-x(ZnO)x solid-solution nanorods can be finely tailored from non-polar {101&cmb.macr;0} to semipolar {101&cmb

  20. Influence of cold stress on contents of soluble sugars, vitamin C and free amino acids including gamma-aminobutyric acid (GABA) in spinach (Spinacia oleracea).

    PubMed

    Yoon, Young-Eun; Kuppusamy, Saranya; Cho, Kye Man; Kim, Pil Joo; Kwack, Yong-Bum; Lee, Yong Bok

    2017-01-15

    The contents of soluble sugars (sucrose, fructose, glucose, maltose and raffinose), vitamin C and free amino acids (34 compounds, essential and non-essential) were quantified in open-field and greenhouse-grown spinaches in response to cold stress using liquid chromatography. In general, greenhouse cultivation produced nutritionally high value spinach in a shorter growing period, where the soluble sugars, vitamin C and total amino acids concentrations, including essential were in larger amounts compared to those grown in open-field scenarios. Further, low temperature exposure of spinach during a shorter growth period resulted in the production of spinach with high sucrose, ascorbate, proline, gamma-aminobutyric acid, valine and leucine content, and these constitute the most important energy/nutrient sources. In conclusion, cultivation of spinach in greenhouse at a low temperature (4-7°C) and exposure for a shorter period (7-21days) before harvest is recommended. This strategy will produce a high quality product that people can eat. PMID:27542466

  1. Encapsulation of ployunsaturated fatty acid esters with solid lipid particles

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Polyunsaturated fatty acids (PUFA) such as a-linolenic acid (ALA) and docosahexaenoic acid (DHA) are known to improve cardiovascular and nervous system health. These compounds are increasingly used in food and animal feed formulations. However, the high degree of unsaturation in these structures can...

  2. Preparation and characterisation of Kolliphor® P 188 and P 237 solid dispersion oral tablets containing the poorly water soluble drug disulfiram.

    PubMed

    Ramadhani, Nisrina; Shabir, Mehwish; McConville, Christopher

    2014-11-20

    The oral route of administration is the most common and preferred route of drug delivery due to its ease of administration, cost-effectiveness and flexibility in design. However, limited aqueous solubility of the active pharmaceutical ingredient can result in poor bioavailability, which is a major issue for the pharmaceutical industry. Increasing numbers of new drugs are falling into class II of the Biopharmaceutical Classification System (BCS), where they have a low solubility and high tissue permeability, meaning that bioavailability is solubility dependent. Here we demonstrate the development and characterisation of solid dispersion oral tablets, containing the poorly water-soluble drug disulfiram, prepared using both the hot melt and solvent evaporation methods and manufactured from two different polymers, Kolliphor(®) P 188 and P 237, specifically designed for the manufacture of solid dispersions. This paper demonstrates that the disulfiram solid dispersions tablets have an enhanced release rate of disulfiram compared to the control tablets. The Kolliphor(®) P 188 polymer control tablets released approximately 48.8% of their disulfiram content over 8h, with the solvent evaporated tablets releasing approximately 65.8%, while the 60 and 80 °C hot melt tablets released approximately 73.2 and 100% of their disulfiram content respectively. A similar trend was seen with Kolliphor(®) P 237 as the control tablets released approximately 50.5% of their disulfiram content over 8h, while the solvent evaporated tablets released approximately 79.5% and the 60 and 80 °C hot melt tablets released 100.2 and 100.3% respectively. Depending on what method and polymer is used to manufacture the solid dispersions the disulfiram is either maintained completely or partially in its amorphous state and it is this which enhances its solubility and release rate from the tablets. The disulfiram in the Kolliphor(®) P 188 solvent evaporated and 60 °C hot melt tablets retained 50

  3. High abundances of water-soluble dicarboxylic acids, ketocarboxylic acids and α-dicarbonyls in the mountain aerosols over the North China Plain during wheat burning season

    NASA Astrophysics Data System (ADS)

    Kawamura, K.; Tachibana, E.; Okuzawa, K.; Aggarwal, S. G.; Kanaya, Y.; Wang, Z. F.

    2013-02-01

    Aerosol (TSP) samples were collected at the summit of Mount Tai (elevation: 1534 m a.s.l., 36.25° N; 117.10° E) located in the North China Plain using a high-volume air sampler and pre-combusted quartz filters. Sampling was conducted on day/night or 3 h basis in the period from 29 May to 28 June 2006 during the field burning of wheat straw residue and the post-burning season. The filter samples were analyzed for low molecular weight dicarboxylic acids, ketoacids and α-dicarbonyls using capillary gas chromatography (GC) and GC-MS employing water extraction and butyl ester derivatization. Dicarboxylic acids (C2-C11, 220-6070 ng m-3) were characterized by a predominance of oxalic (C2) acid (105-3920 ng m-3) followed by succinic (C4) or malonic (C3) acid. Unsaturated aliphatic diacids, including maleic (M), isomaleic (iM) and fumaric (F) acid, were also detected together with aromatic diacids (phthalic, iso-phthalic and tere-phthalic acids). ω-Oxocarboxylic acids (C2-C9, 24-610 ng m-3) were detected as the second most abundant compound class with the predominance of glyoxylic acid (11-360 ng m-3), followed by α-ketoacid (pyruvic acid, 3-140 ng m-3) and α-dicarbonyls (glyoxal, 1-230 ng m-3 and methylglyoxal, 2-120 ng m-3). We found that these levels (> 6000 ng m-3 for diacids) are several times higher than those reported in Chinese megacities at ground levels. The concentrations of diacids increased from late May to early June showing a maximum on 7 June and then significantly decreased during 8-11 June when the wind direction shifted from northeasterly to northerly. Similar temporal trends were found for ketocarboxylic acids and α-dicarbonyls as well as total carbon (TC) and water-soluble organic carbon (WSOC). The temporal variations of water-soluble organics were interpreted by the direct emission from the field burning products of agricultural wastes (wheat straw) in the North China Plain and the subsequent photochemical oxidation of volatile and semi

  4. The effect of low solubility organic acids on the hygroscopicity of sodium halide aerosols

    NASA Astrophysics Data System (ADS)

    Miñambres, L.; Méndez, E.; Sánchez, M. N.; Castaño, F.; Basterretxea, F. J.

    2014-10-01

    In order to accurately assess the influence of fatty acids on the hygroscopic and other physicochemical properties of sea salt aerosols, hexanoic, octanoic or lauric acid together with sodium halide salts (NaCl, NaBr and NaI) have been chosen to be investigated in this study. The hygroscopic properties of sodium halide sub-micrometre particles covered with organic acids have been examined by Fourier-transform infrared spectroscopy in an aerosol flow cell. Covered particles were generated by flowing atomized sodium halide particles (either dry or aqueous) through a heated oven containing the gaseous acid. The obtained results indicate that gaseous organic acids easily nucleate onto dry and aqueous sodium halide particles. On the other hand, scanning electron microscopy (SEM) images indicate that lauric acid coating on NaCl particles makes them to aggregate in small clusters. The hygroscopic behaviour of covered sodium halide particles in deliquescence mode shows different features with the exchange of the halide ion, whereas the organic surfactant has little effect in NaBr particles, NaCl and NaI covered particles experience appreciable shifts in their deliquescence relative humidities, with different trends observed for each of the acids studied. In efflorescence mode, the overall effect of the organic covering is to retard the loss of water in the particles. It has been observed that the presence of gaseous water in heterogeneously nucleated particles tends to displace the cover of hexanoic acid to energetically stabilize the system.

  5. Characterization of a soluble phosphatidic acid phosphatase in bitter melon (Momordica charantia)

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Momordica charantia is often called bitter melon, bitter gourd or bitter squash because its fruit has a bitter taste. The fruit has been widely used as vegetable and herbal medicine. Alpha-eleostearic acid is the major fatty acid in the seeds, but little is known about its biosynthesis. As an initia...

  6. Solvent-Free Polymerization of L-Aspartic Acid in the Presence of D-Sorbitol to Obtain Water Soluble or Network Copolymers

    Technology Transfer Automated Retrieval System (TEKTRAN)

    L-aspartic acid was thermally polymerized in the presence of D-sorbitol with the goal of synthesizing new, higher molecular weight water soluble and absorbent copolymers. No reaction occurred when aspartic acid alone was heated at 170 or 200 degrees C. In contrast, heating sorbitol and aspartic ac...

  7. Application of the solid dispersion method to the controlled release of medicine. IV. Precise control of the release rate of a water soluble medicine by using the solid dispersion method applying the difference in the molecular weight of a polymer.

    PubMed

    Yuasa, H; Ozeki, T; Kanaya, Y; Oishi, K

    1993-05-01

    Solid dispersions were prepared by the evaporation of ethanol after dissolving into ethanol a water soluble medicine (oxprenolol hydrochloride (OXP)), four grades of water insoluble ethylcellulose (EC) and four grades of water soluble hydroxypropyl cellulose (HPC), both having different molecular weights. The precise control of the release rat of a water soluble medicine by applying the difference in the molecular weight of polymers was attempted. The pore size distribution in solid dispersion granules was measured before and after the dissolution test by mercury intrusion porosimetry to clarify the mechanism of medicine release from the granules when the molecular weights of polymers were different. The state of medicine in the solid dispersions was analyzed by thermal analysis and X-ray diffractometry. Although the difference was slight, the release rate of OXP from the granules of the OXP-HPC system decreased as the molecular weight of HPC increased. The release behavior of OXP in the OXP-EC system was scarcely affected by the molecular weight of EC. However, in the OXP-EC-HPC system, the release rate markedly decreased with a larger molecular weight of EC. It was thought from the results of the pore size distribution that there were two types of release routes for OXP; dissolving directly into the dissolution medium and diffusing in the swelled HPC phase, caused by the addition of HPC. The decrease in the release rate of OXP in the OXP-EC-HPC system was caused by the increase in the ratio of OXP dissolving via the latter route, occurring with a larger molecular weight of EC. These results suggest that it is feasible to precisely control the release of a water soluble medicine by varying the molecular weight of the polymers in the solid dispersion. PMID:8339340

  8. Solid solubility of rare earth elements (Nd, Eu, Tb) in In2-xSnxO3 - effect on electrical conductivity and optical properties.

    PubMed

    Sunde, T O L; Lindgren, M; Mason, T O; Einarsrud, M-A; Grande, T

    2014-07-01

    Wide band-gap semiconductors doped with luminescent rare earth elements (REEs) have attracted recent interest due to their unique optical properties. Here we report on the synthesis of the transparent conducting oxides (TCOs) indium oxide and indium tin oxide (ITO) doped with neodymium, europium and terbium. The solid solubility in the systems was investigated and isothermal phase diagrams at 1400 °C were proposed. The solubility of the REEs in In2O3 is mainly determined by the size of the rare earth dopant, while in ITO the solid solubility was reduced due to a strong tendency of the tin and REE co-dopants to form a pyrochlore phase. The effect of the REE-doping on the conductivity of the host was determined and optical activity of the REE dopants were investigated in selected host materials. The conductivity of sintered materials of REE-doped In2O3 was significantly reduced, even at small doping concentrations, due to a decrease in carrier mobility. The same decrease in mobility was not observed in thin films of the material processed at lower temperatures. Strong emissions at around 611 nm were observed for Eu-doped In2O3, demonstrating the possibility of obtaining photoluminescence in a TCO host, while no emissions was observed for Nd- and Tb-doping. PMID:24832103

  9. Extended chain conformational preference of solid films of poly(2,6-benzoxazole) processed from Lewis acid coordination complexes

    SciTech Connect

    Chen, X.L.; Jenekhe, S.A.

    1996-12-31

    Polybenzoxazoles such as poly(2,6-benzoxazole)(2,6-PBO), poly(2,6-benzothiazole)(2,6-PBT) and poly(2,5(6)-benzimidazole) are semi-flexible, high temperature, and high modulus polymers which have been of wide interest as the matrix components of molecular composites. These polymers and their rigid-rod relatives polybenzobisazoles(PBZT, PBO, etc) also exhibit interesting electroactive and photoactive properties. As previously shown for rigid-rod polybenzobisazoles, we have found that the semi-flexible polybenzoazoles are soluble in Lewis acid (e.g. GaCl{sub 3}, AlCl{sub 3})/nitromethane solvent systems from which films and fibers could be processed. Remarkably, 2,6-PBO films prepared by complexation mediated processing from Lewis acid/nitromethane solutions of the polymer exhibit the extended chain (trans) conformation as evidenced by optical absorption and photoluminescence spectroscopies. In contrast, 2,6-PBO films prepared from formic acid/methanesulfonic acid(FA/MSA) solvent am predominantly of cis-conformation. The origin of this extended chain conformation preference of 2,6-PBO films prepared from Lewis acid/nitromethane solutions lies in the stereochemical control exerted by Lewis(MX{sub 3}) coordination to the imine nitrogens of 2,6-PBO resulting in an all-trans conformation after film processing and decomplexation. Since the trans- and cis-(2,6-PBO) have dramatically different solid state properties such as optical absorption and luminescence, our results demonstrate how a high degree of control of solid state structure and properties can be achieved by novel polymer processing.

  10. A Mini-Review on Solid Acid Catalysts for Esterification Reactions

    NASA Astrophysics Data System (ADS)

    Sirsam, Rajkumar; Hansora, Dharmesh; Usmani, Ghayas A.

    2016-04-01

    This paper presents an overview of research pertaining to solid acid catalysts for esterification reactions. Prominence has been given to the literatures that have been appeared during the last two decades. A variety of reactions catalyzed by solid acid catalysts have been tabulated according to their broad classification; industrially important reactions have been outlined. Examples, where the use of various solid acid catalysts have led to an improvement in the selectivity of the desired products, have also been discussed. Various catalyzed esterification reactions using different approaches and previous kinetic studies have been reviewed. Types, preparation and synthesis of various solid acid catalysts have been reviewed and discussed. Suggestions have been summarized for their implementation in future work.

  11. Radiation-induced reactions of amino acids adsorbed on solid surfaces

    NASA Astrophysics Data System (ADS)

    López-Esquivel Kranksith, L.; Negrón-Mendoza, A.; Mosqueira, F. G.; Ramos-Bernal, Sergio

    2010-07-01

    The purpose of this work is to study the adsorption of compounds such as amino acids on clays and carbon nanotubes (CNTs) as a possible phase in the chemical evolution that may have occurred on the primitive Earth or in extraterrestrial environments. We further study the behavior of amino acids adsorbed on these solid surfaces at different conditions of pH and levels of irradiation, simulating a high-radiation field at early Earth conditions. The relevance of this work is to explain the possible contribution of solids (clays and CNTs) as promoters of polymerization and as shields for the adsorbed organic compounds against external sources of energy. To this end, tryptophan, aspartic acid, and glutamic acid were adsorbed on fixed amounts of solid surfaces and were irradiated by a 60Co source for different periods of time at fixed dose rates. After irradiation, the amino acids were extracted from the solid and analyzed with UV and IR spectroscopes and high-performance liquid chromatography. The most efficient surface for adsorption of amino acids was clay, followed by CNTs. Studies of the gamma irradiation of amino acids adsorbed on clay (in the solid phase) show a low yield of recovery of the amino acid.

  12. Aircraft observations of water-soluble dicarboxylic acids in the aerosols over China

    NASA Astrophysics Data System (ADS)

    Zhang, Yan-Lin; Kawamura, Kimitaka; Qing Fu, Ping; Boreddy, Suresh K. R.; Watanabe, Tomomi; Hatakeyama, Shiro; Takami, Akinori; Wang, Wei

    2016-05-01

    Vertical profiles of dicarboxylic acids, related organic compounds and secondary organic aerosol (SOA) tracer compounds in particle phase have not yet been simultaneously explored in East Asia, although there is growing evidence that aqueous-phase oxidation of volatile organic compounds may be responsible for the elevated organic aerosols (OA) in the troposphere. Here, we found consistently good correlation of oxalic acid, the most abundant individual organic compounds in aerosols globally, with its precursors as well as biogenic-derived SOA compounds in Chinese tropospheric aerosols by aircraft measurements. Anthropogenically derived dicarboxylic acids (i.e., C5 and C6 diacids) at high altitudes were 4-20 times higher than those from surface measurements and even occasionally dominant over oxalic acid at altitudes higher than 2 km, which is in contrast to the predominance of oxalic acid previously reported globally including the tropospheric and surface aerosols. This indicates an enhancement of tropospheric SOA formation from anthropogenic precursors. Furthermore, oxalic acid-to-sulfate ratio maximized at altitudes of ˜ 2 km, explaining aqueous-phase SOA production that was supported by good correlations with predicted liquid water content, organic carbon and biogenic SOA tracers. These results demonstrate that elevated oxalic acid and related SOA compounds from both the anthropogenic and biogenic sources may substantially contribute to tropospheric OA burden over polluted regions of China, implying aerosol-associated climate effects and intercontinental transport.

  13. Formation of water-soluble dicarboxylic acids, oxoacids and a-dicarbonyls by ozone oxidation of isoprene

    NASA Astrophysics Data System (ADS)

    Kawamura, K.; Tachibana, E.; Sakamoto, Y.; Hirokawa, J.

    2014-12-01

    Water-soluble dicarboxylic acids such as oxalic acid (C2) are the dominant organic compound class in atmospheric aerosols. They can act as cloud condensation nuclei and affect on the Earth climate. Diacids can be primary emitted from fossil fuel combustion and biomass burning and secondarily produced by photochemical oxidations of biogenic and anthropogenic hydrocarbons. However, their sources and formation processes are still not well understood. Recently model and observation studies suggested the importance of isoprene as a precursor of oxalic acid. Isoprene is the most abundant BVOC emitted from terrestrial plants and can serve as important precursors of diacids. We conducted a laboratory oxidation of isoprene (2.0 ppm) with ozone (4.3 ppm) in a Teflon bag for 10 to 480 min. The formed particles were collected with quartz fiber filters and analyzed for diacids, oxoacids and a-dicarbonyls employing water extraction and butyl ester derivatization and using GC and GC/MS techniques. Here, we report the analytical results to better understand the formation process of diacids and related compounds from isoprene. We detected homologous series of saturated diacids (C2-C6), unsaturated diacids (maleic and methylmaleic acids), w-oxocarboxylic acids (C2-C9), pyruvic acid, glyoxal and methylglyoxal. We found that oxalic acid (3000-9700 ngm-3) is the most abundant diacid followed by succinic (C4) or malonic (C3) acid. Their concentrations increased with reaction time showing a maximum in 4 hours. Interestingly, C3/C4 ratios increased with time. The second most abundant species after oxalic acid was generally methylglyoxal (3600-9600 ngm-3), except for the 30 min. sample where methylglyoxal was more abundant than oxalic acid. Glyoxylic acid (wC2) was found as the most abundant oxoacid (1600-3800 ngm-3) followed by wC3 and wC4. Although the concentrations of diacids and related compounds are 1-2 orders magnitude higher than those reported in ambient aerosols, this study

  14. Conversion of solid dispersion prepared by acid-base interaction into free-flowing and tabletable powder by using Neusilin® US2.

    PubMed

    Shah, Ankita; Serajuddin, Abu T M

    2015-04-30

    A novel method of greatly increasing solubility and dissolution rate of a model basic drug, haloperidol, by interacting it with water-soluble weak organic acids in aqueous media was previously reported in the literature. Amorphous solid dispersion (SD) was formed when solutions containing haloperidol and various acids were dried. However, the SDs were semisolid, viscous and sticky, especially when the drug load was high, and could not be processed into tablets. The drug release from SD was also incomplete since the viscous material did not readily mix with aqueous media. In the present study, a mesoporous metalosilicate, Neusilin(®) US2, was incorporated in SDs prepared by using malic, tartaric and citric acids. The silicate constituted 40% w/w of the total solid mass. The addition of silicate converted SDs into powders, which were then characterized for flow properties, bulk and tap density, and tabletability. Their physical properties were found to be acceptable for the development of tablets. DSC and powder XRD showed that haloperidol and acids converted completely to amorphous forms, and they did not show any sign of crystallization during accelerated stability study at 40°C/75% RH and 25°C/60% RH for 9 months. Complete drug release under gastrointestinal pH conditions could be obtained from tablets prepared. PMID:25724137

  15. Defensive strategies in Geranium sylvaticum, Part 2: Roles of water-soluble tannins, flavonoids and phenolic acids against natural enemies.

    PubMed

    Tuominen, Anu

    2013-11-01

    Geranium sylvaticum is a common herbaceous plant in Fennoscandia, which has a unique phenolic composition. Ellagitannins, proanthocyanidins, galloylglucoses, gallotannins, galloyl quinic acids and flavonoids possess variable distribution in its different organs. These phenolic compounds are thought to have an important role in plant-herbivore interactions. The aim of this study was to quantify these different water-soluble phenolic compounds and measure the biological activity of the eight organs of G. sylvaticum. Compounds were characterized and quantified using HPLC-DAD/MS, in addition, total proanthocyanidins were determined by BuOH-HCl assay and total phenolics by the Folin-Ciocalteau method. Two in vitro biological activity measurements were used: the prooxidant activity was measured by the browning assay and antioxidant activity by the 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging assay. Organ extracts were fractionated using column chromatography on Sephadex LH-20 and the activities of fractions was similarly measured to evaluate which polyphenol groups contributed the most to the biological activity of each organ. The data on the activity of fractions were examined by multivariate data analysis. The water-soluble extracts of leaves and pistils, which contained over 30% of the dry weight as ellagitannins, showed the highest pro-oxidant activity among the organ extracts. Fraction analysis revealed that flavonoids and galloyl quinic acids also exhibited high pro-oxidant activity. In contrast, the most antioxidant active organ extracts were those of the main roots and hairy roots that contained high amounts of proanthocyanidins in addition to ellagitannins. Analysis of the fractions showed that especially ellagitannins and galloyl quinic acids have high antioxidant activity. We conclude that G. sylvaticum allocates a significant amount of tannins in those plant parts that are important to the fitness of the plant and susceptible to natural enemies, i

  16. Solubility and equilibrium vapor pressures of HC1 dissolved in polar stratospheric cloud materials - Ice and the trihydrate of nitric acid

    NASA Technical Reports Server (NTRS)

    Hanson, David; Mauersberger, Konrad

    1988-01-01

    Measurements of the pressure-solubility behavior of HC1 in water ice and in the nitric acid trihydrate (NAT) crystal at 200 K are reported. It was found that HC1 is about 20 times more soluble in NAT than in ice for stratospheric conditions. A relation between HC1 pressure and substrate composition based on the Gibbs-Duhem equation is developed. This relation, along with other thermodynamic data, can be used to obtain the HC1 pressure-solubility behavior at different temperatures. Implications of these results for the south polar ozone hole are discussed.

  17. Reactivity of Water Soluble Organic Acids with Chloride and Nitrate Particles Investigated by Micro-spectroscopy Analysis

    NASA Astrophysics Data System (ADS)

    Wang, B.; OBrien, R. E.; Kelly, S. T.; Shilling, J. E.; Tivanski, A.; Moffet, R.; Gilles, M. K.; Laskin, A.

    2013-12-01

    Atmospheric particles often consist of a complex organic and inorganic mixture. Interactions between organic and inorganic species may affect particles' chemical and physical properties thus atmospheric chemistry and climate. Water soluble organic acids (WSOA) can contribute a significant fraction of organic materials in condense phase. Inorganic particles, such as sea salt and mineral dust, are main components in the atmosphere and can undergo complex heterogeneous reactions. For example, depletion of chloride in sea salt particles was reported in previous field studies and was attributed to the acid displacement of chlorides with inorganic acids, such as nitric and sulfuric acids. Recently, we showed that NaCl can react with WSOA resulting in the release gaseous HCl and formation of organic salts. A similar mechanism is also applicable to mixed WSOA/nitrate particles where acid displacement reactions are mainly driven by the high volatility and evaporation of HNO3 as particles go through dehydration process. Furthermore, secondary organic material (SOM), which contains a complex mixture of carboxylic acids, exhibits a similar reactivity towards chlorides and nitrates. Here, we present field and laboratory studies on the reactions between atmospheric relevant WSOA/SOM and inorganic salts including NaCl, NaNO3, and Ca(NO3)2 using complementary micro-spectroscopy analysis such as computer controlled scanning electron microscopy with energy dispersive analysis of X-rays (CCSEM/EDX), scanning transmission X-ray microscopy with near edge X-ray absorption fine structure spectroscopy (STXM/NEXAFS), and micro-Fourier transform infrared spectroscopy (micro-FTIR). The results show various potentials of chloride and nitrate depletion by WSOA and SOM. Formation of corresponding organic salts is confirmed and quantified.

  18. Pretreatment of dried distillers grains with solubles by soaking in aqueous ammonia and subsequent enzymatic/dilute acid hydrolysis to produce fermentable sugars

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Dried distillers grains with solubles (DDGS), a co-product of corn ethanol production in the dry-grind process, was pretreated by soaking in aqueous ammonia (SAA) using a 15% w/w NH4OH solution at a solid:liquid ratio of 1:10. The effect of pretreatment on subsequent enzymatic hydrolysis was studied...

  19. Release of a Poorly Soluble Drug from Hydrophobically Modified Poly (Acrylic Acid) in Simulated Intestinal Fluids

    PubMed Central

    Knöös, Patrik

    2015-01-01

    A large part of new pharmaceutical substances are characterized by a poor solubility and high hydrophobicity, which might lead to a difference in drug adsorption between fasted and fed patients. We have previously evaluated the release of hydrophobic drugs from tablets based on Pemulen TR2 and showed that the release can be manipulated by adding surfactants. Here we further evaluate the possibility to use Pemulen TR2 in controlled release tablet formulations containing a poorly soluble substance, griseofulvin. The release is evaluated in simulated intestinal media that model the fasted state (FaSSIF medium) or fed state (FeSSIF). The rheology of polymer gels is studied in separate experiments, in order to gain more information on possible interactions. The release of griseofulvin in tablets without surfactant varied greatly and the slowest release were observed in FeSSIF. Addition of SDS to the tablets eliminated the differences and all tablets showed a slow linear release, which is of obvious relevance for robust drug delivery. Comparing the data from the release studies and the rheology experiment showed that the effects on the release from the different media could to a large extent be rationalised as a consequence of the interactions between the polymer and the surfactants in the media. The study shows that Pemulen TR2 is a candidate for controlled release formulations in which addition of surfactant provides a way to eliminate food effects on the release profile. However, the formulation used needs to be designed to give a faster release rate than the tablets currently investigated. PMID:26473964

  20. Release of a Poorly Soluble Drug from Hydrophobically Modified Poly (Acrylic Acid) in Simulated Intestinal Fluids.

    PubMed

    Knöös, Patrik; Svensson, Anna V; Ulvenlund, Stefan; Wahlgren, Marie

    2015-01-01

    A large part of new pharmaceutical substances are characterized by a poor solubility and high hydrophobicity, which might lead to a difference in drug adsorption between fasted and fed patients. We have previously evaluated the release of hydrophobic drugs from tablets based on Pemulen TR2 and showed that the release can be manipulated by adding surfactants. Here we further evaluate the possibility to use Pemulen TR2 in controlled release tablet formulations containing a poorly soluble substance, griseofulvin. The release is evaluated in simulated intestinal media that model the fasted state (FaSSIF medium) or fed state (FeSSIF). The rheology of polymer gels is studied in separate experiments, in order to gain more information on possible interactions. The release of griseofulvin in tablets without surfactant varied greatly and the slowest release were observed in FeSSIF. Addition of SDS to the tablets eliminated the differences and all tablets showed a slow linear release, which is of obvious relevance for robust drug delivery. Comparing the data from the release studies and the rheology experiment showed that the effects on the release from the different media could to a large extent be rationalised as a consequence of the interactions between the polymer and the surfactants in the media. The study shows that Pemulen TR2 is a candidate for controlled release formulations in which addition of surfactant provides a way to eliminate food effects on the release profile. However, the formulation used needs to be designed to give a faster release rate than the tablets currently investigated. PMID:26473964

  1. Clay Minerals as Solid Acids and Their Catalytic Properties.

    ERIC Educational Resources Information Center

    Helsen, J.

    1982-01-01

    Discusses catalytic properties of clays, attributed to acidity of the clay surface. The formation of carbonium ions on montmorillonite is used as a demonstration of the presence of surface acidity, the enhanced dissociation of water molecules when polarized by cations, and the way the surface can interact with organic substances. (Author/JN)

  2. Non-invasive insight into the release mechanisms of a poorly soluble drug from amorphous solid dispersions by confocal Raman microscopy.

    PubMed

    Punčochová, Kateřina; Vukosavljevic, Branko; Hanuš, Jaroslav; Beránek, Josef; Windbergs, Maike; Štěpánek, František

    2016-04-01

    In this study, we investigated the release mechanism of the poorly water soluble drug aprepitant from different amorphous solid dispersions using confocal Raman microscopy (CRM). Solid dispersions were fabricated based on either Soluplus®, as an amphiphilic copolymer and solubilizer, or on polyvinylpyrrolidone, as a hydrophilic polymer, in order to elucidate the influence of the polymer characteristics on the drug form and dissolution mechanisms. Aprepitant exhibited its amorphous form in both solid dispersions. However, the release differed depending on the polymer. The high complexation effect of Soluplus was shown to be a crucial factor for stabilization of the amorphous drug, resulting in continuous release without any recrystallization of aprepitant. In contrast, solid dispersions based on polyvinylpyrrolidone showed a different mechanism of dissolution; due to the good affinity of PVP and water, the polymer is dissolving fast, leading to phase separation and local recrystallization of the drug. The study highlights the complexity of release processes from solid dispersions and elucidates the influence of the polymer on drug release kinetics. PMID:26861928

  3. The role of small acid-soluble proteins (SASPs) in protection of spores of Clostridium botulinum against nitrous acid.

    PubMed

    Meaney, Carolyn A; Cartman, Stephen T; McClure, Peter J; Minton, Nigel P

    2016-01-01

    Mutant strains of Clostridium botulinum ATCC 3502 were generated using the ClosTron in four genes (CBO1789, CBO1790, CBO3048, CBO3145) identified as encoding α/β-type SASP homologues. The spores of mutant strains in which CBO1789 or CBO1790 was inactivated demonstrated a significant increase in sensitivity to the damaging agent nitrous acid (P<0.01), a phenotype that was partially restored to wild-type in complementation studies. In contrast to nitrous acid, the spores of the CBO1789 and CBO1790 mutants showed no change in their resistance to formaldehyde and hydrogen peroxide (P>0.05), two other chemicals commonly used as components of disinfection regimes. These data indicate that the SASPs CBO1789 or CBO1790 play a significant role in resistance to nitrous acid, but not in resistance to formaldehyde or hydrogen peroxide. PMID:26386202

  4. J-aggregation of a water-soluble tetracationic porphyrin in mixed LB films with a calix[8]arene carboxylic acid derivative.

    PubMed

    Miguel, Gustavo de; Pérez-Morales, Marta; Martín-Romero, María T; Muñoz, Eulogia; Richardson, Tim H; Camacho, Luis

    2007-03-27

    The molecular organization of a mixed film, containing a water-soluble tetracationic porphyrin (TMPyP) and a p-tert-butyl calix[8]arene octacarboxylic acid derivative (C8A), at the air-water interface and on a solid support (LB film), has been investigated. Although the TMPyP aggregation was not detected at the air-water interface, TMPyP J-aggregates have been found in the LB films (Y-type). Unlike tetraanionic porphyrins, for example TSPP, the TMPyP J-aggregates are not induced by a zwitterion formation. The TMPyP J-aggregation is a result of a "double comb" configuration, where porphyrins from opposite layers are interwoven in a linear infinite J-aggregate. Our results confirm that TMPyP molecules tend to self-aggregate strongly, provided the electrostatic repulsions of their peripheral groups are cancelled by the anionic groups of the C8A matrix. PMID:17315895

  5. Water-Soluble Poly(p-aryleneethynylene)s: A Sensor Array Discriminates Aromatic Carboxylic Acids.

    PubMed

    Han, Jinsong; Wang, Benhua; Bender, Markus; Seehafer, Kai; Bunz, Uwe H F

    2016-08-10

    A chemical tongue consisting of 11 elements (four poly(p-aryleneethynylene)s (PAE) at pH 7 and pH 13, and seven electrostatic complexes formed from oppositely charged poly(p-aryleneethynylene)s at pH 7) discriminate 21 benzoic and phenylacetic acid derivatives in aqueous solution. The mechanism of discrimination is the fluorescence modulation of the PAEs, leading to quenching or fluorescence turn-on. The PAEs alone at both pH values and the tongue, consisting of the complexes only, discriminate the 21 acids with 92% (PAEs at pH 7), 95% (PAEs at pH 13), and 99% (complexes at pH 7) reliability after linear discriminant analysis (LDA). A sensor field with all 14 elements, according to LDA, discriminates all of the 21 acids with 100% accuracy. PMID:27415439

  6. Solid solubility, phase transitions, thermal expansion, and compressibility in Sc{sub 1−x}Al{sub x}F{sub 3}

    SciTech Connect

    Morelock, Cody R.; Gallington, Leighanne C.; Wilkinson, Angus P.

    2015-02-15

    With the goal of thermal expansion control, the synthesis and properties of Sc{sub 1−x}Al{sub x}F{sub 3} were investigated. The solubility limit of AlF{sub 3} in ScF{sub 3} at ∼1340 K is ∼50%. Solid solutions (x≤0.50) were characterized by synchrotron powder diffraction at ambient pressure between 100 and 900 K and at pressures <0.414 GPa while heating from 298 to 523 K. A phase transition from cubic to rhombohedral is observed. The transition temperature increases smoothly with Al{sup 3+} content, approaching 500 K at the solid solubility limit, and also upon compression at fixed Al{sup 3+} content. The slope of the pressure–temperature phase boundary is ∼0.5 K MPa{sup −1}, which is steep relative to that for most symmetry-lowering phase transitions in perovskites. The volume coefficient of thermal expansion (CTE) for the rhombohedral phase is strongly positive, but the cubic-phase CTE varies from negative (x<0.15) to near-zero (x=0.15) to positive (x>0.20) between ∼600 and 800 K. The cubic solid solutions elastically stiffen on heating, while Al{sup 3+} substitution causes softening at a given temperature. - Graphical abstract: The cubic-phase coefficient of thermal expansion for Sc{sub 1−x}Al{sub x}F{sub 3}(solubility limit ∼50% at ∼1340 K) becomes more positive with increased Al{sup 3+} substitution, but the average isothermal bulk modulus decreases (elastic softening). - Highlights: • The solubility limit of AlF{sub 3} in ScF{sub 3} at ∼1340 K is ∼50%. • The phase transition temperature of Sc{sub 1−x}Al{sub x}F{sub 3} increases smoothly with x. • The cubic-phase volume CTE varies from negative to positive with increasing x. • The cubic solid solutions elastically stiffen on heating. • Al{sup 3+} substitution causes softening at a given temperature.

  7. Cotton wool-like poly(lactic acid)/vaterite composite scaffolds releasing soluble silica for bone tissue engineering.

    PubMed

    Obata, Akiko; Ozasa, Hiroki; Kasuga, Toshihiro; Jones, Julian R

    2013-07-01

    Cotton wool-like poly(L-lactic acid) and siloxane-doped vaterite (SiV) composite scaffolds were prepared with a modified electrospinning system for bone tissue engineering applications. The effects of changing the SiV content in the materials from 10 to 30 wt% on elasticity and the ability to release calcium ions and soluble silica were evaluated. The elasticity of the cotton wool-like composites was almost the same as that of the PLLA from the results of compressibility and recovery tests. The materials released calcium ions for more than 56 days and soluble silica for 28-56 days in a tris buffer solution (pH 7.4). Mouse osteoblast-like cells (MC3T3-E1 cells) were cultured on/in the cotton wool-like materials or the fibremats out of the same composite materials as that used for the cotton wool-like materials. The cells penetrated into and proliferated inside the cotton wool-like materials, although they mainly adhered on the fibremat surface. PMID:23606191

  8. Preparation and physicochemical properties of soluble dietary fiber from orange peel assisted by steam explosion and dilute acid soaking.

    PubMed

    Wang, Lei; Xu, Honggao; Yuan, Fang; Fan, Rui; Gao, Yanxiang

    2015-10-15

    The coupled pretreatment of orange peel with steam explosion (SE) and sulfuric-acid soaking (SAS) was investigated to enhance the yield and improve the functionality of soluble dietary fiber (SDF). When orange peel was pretreated by SE at 0.8MPa for 7 min, combined with 0.8% SAS, the content of SDF was increased from 8.04% to 33.74% in comparison to the control and SDF prepared with SE-SAS showed the high water solubility, water-holding capacity, oil-holding capacity, swelling capacity, emulsifying activity, emulsion stability and foam stability. SDF from orange peel treated by SE-SAS exhibited significantly (p < 0.05) higher binding capacity for three toxic cations (Pb, As and Cu) and smaller molecular weight (Mw = 174 kDa). Furthermore, differential scanning calorimetry (DSC) measurement showed that SDF from orange peel treated by SE-SAS had a higher peak temperature (170.7 ± 0.4 °C) than that of the untreated sample (163.4 ± 0.3 °C). Scanning electron micrograph (SEM) images demonstrated that the surface of SDF from orange peel treated by SE-SAS was rough and collapsed. It can be concluded that SDF from orange peel treated by SE-SAS has the higher potential to be applied as a functional ingredient in food products. PMID:25952845

  9. Hygroscopic properties of ultrafine aerosol particles in the boreal forest: diurnal variation, solubility and the influence of sulfuric acid

    NASA Astrophysics Data System (ADS)

    Ehn, M.; Petäjä, T.; Aufmhoff, H.; Aalto, P.; Hämeri, K.; Arnold, F.; Laaksonen, A.; Kulmala, M.

    2006-10-01

    Freshly formed atmospheric aerosol particles are neither large enough to efficiently scatter incoming solar radiation nor able to act as cloud condensation nuclei. As the particles grow larger, their hygroscopicity determines the limiting size after which they are important in both of the aforementioned processes. The condensing species resulting in growth alter the hygroscopicity of the particles. We have measured hygroscopic growth of aerosol particles present in a boreal forest, along with the very hygroscopic atmospheric trace gas sulfuric acid. The focus was on days with new particle formation by nucleation. The measured hygroscopic growth factors (GF) correlated positively with gaseous phase sulfuric acid concentrations. This correlation had a strong size dependency; the smaller the particle, the more condensing sulfuric acid is bound to alter the GF due to initially smaller mass. In addition, water uptake of nucleation mode particles was monitored during new particle formation events and followed during their growth to Aitken mode sizes. As the modal diameter increased, the solubility of the particles decreased. This indicated that initially more hygroscopic particles transformed into less hygroscopic or even hydrophobic particles. A similar behavior was seen also during days with no particle formation, with GF decreasing during the evenings and increasing during early morning. This can be tentatively explained by day- and nighttime differences in the hygroscopicity of condensable vapors.

  10. Prevention of bovine mastitis by a postmilking teat disinfectant containing chlorous acid and chlorine dioxide in a soluble polymer gel.

    PubMed

    Oliver, S P; King, S H; Torre, P M; Shull, E P; Dowlen, H H; Lewis, M J; Sordillo, L M

    1989-11-01

    A natural exposure study was conducted in a herd of 150 lactating dairy cows for 18 mo to determine the effectiveness of chlorous acid and chlorine dioxide in a soluble polymer gel as a postmilking teat disinfectant for the prevention of bovine mastitis. Right quarters of cows were dipped in the experimental teat dip after milking machine removal. Left quarters were not dipped and served as within-cow negative controls. The experimental teat dip reduced Staphylococcus aureus infections 67.4%, Streptococcus dysgalactiae infections 63.8%, and Streptococcus uberis infections 27.8%. Overall efficacy of the chlorous acid and chlorine dioxide teat dip against major mastitis pathogens was 52.2%. The experimental teat dip reduced Corynebacterium bovis infections and coagulase-negative staphylococcal infections also by 45.8 and 38.7%, respectively. Overall efficacy against minor mastitis pathogens was 43.4%. Under conditions of this trial, the experimental teat dip containing chlorous acid and chlorine dioxide was effective in preventing new intramammary infections against a variety of mastitis pathogens. PMID:2625499

  11. Fatty acids and fat-soluble vitamins in ewe's milk predicted by near infrared reflectance spectroscopy. Determination of seasonality.

    PubMed

    Revilla, I; Escuredo, O; González-Martín, M I; Palacios, C

    2017-01-01

    The aim of the present work was to determine the fatty acid and fat-soluble vitamin composition and the season of ewe's milk production using NIR spectroscopy. 219 ewe's milk samples from different breeds and feeding regimes were taken each month over one year. Fatty acids were analyzed by gas chromatography, and retinol and α-, and γ-tocopherol by liquid chromatography. The results showed that the quantification was more accurate for the milk dried on paper, except for vitamins. Calibration statistical descriptors on milk dried on paper were good for capric, lauric, myristic, palmitoleic, stearic and oleic acids, and acceptable for caprilic, undecanoic, 9c, 11tCLA, ΣCLA, PUFA, ω3, ω6, retinol and α-tocopherol. The equations for the discrimination of seasonality was obtained using the partial least squares discriminant analysis (PLSDA) algorithm. 93% of winter samples and 89% of summer samples were correctly classified using the NIR spectra of milk dried on paper. PMID:27507500

  12. Boronic acid as an efficient anchor group for surface modification of solid polyvinyl alcohol.

    PubMed

    Nishiyabu, Ryuhei; Shimizu, Ai

    2016-07-28

    We report the use of boronic acid as an anchor group for surface modification of solid polyvinyl alcohol (PVA); the surfaces of PVA microparticles, films, and nanofibers were chemically modified with boronic acid-appended fluorescent dyes through boronate esterification using a simple soaking technique in a short time under ambient conditions. PMID:27311634

  13. Phytase activity of lactic acid bacteria and their impact on the solubility of minerals from wholemeal wheat bread.

    PubMed

    Cizeikiene, Dalia; Juodeikiene, Grazina; Bartkiene, Elena; Damasius, Jonas; Paskevicius, Algimantas

    2015-01-01

    The objective of this study was to determinate phytase activity of bacteriocins producing lactic acid bacteria previously isolated from spontaneous rye sourdough. The results show that the highest extracellular phytase activity produces Pediococcus pentosaceus KTU05-8 and KTU05-9 strains with a volumetric phytase activity of 32 and 54 U/ml, respectively, under conditions similar to leavening of bread dough (pH 5.5 and 30 °C). In vitro studies in simulated gastrointestinal tract media pH provide that bioproducts prepared with P. pentosaceus strains used in wholemeal wheat bread preparation increase solubility of iron, zinc, manganese, calcium and phosphorus average 30%. Therefore, P. pentosaceus KTU05-9 and KTU05-8 strains could be recommended to use as a starter for sourdough preparation for increasing of mineral bioavailability from wholemeal wheat bread. PMID:26397032

  14. Single-walled carbon nanotubes in strong acids: controlling solubility and the liquid crystal phase.

    NASA Astrophysics Data System (ADS)

    Pasquali, Matteo

    2006-03-01

    Single Walled Nanotubes (SWNTs have remarkable electrical, thermal, and mechanical properties. Neat, well-aligned SWNT fibers and sheets could be the ultimate building blocks of strong, ultra-light multifunctional materials for aerospace applications, and could yield electromechanical actuators and sensors with unprecedented performance. After the achievement of scalable production of SWNTs, the difficulty of processing pristine SWNTs by liquid-phase methods has been the single most important roadblock to manufacturing macroscopic materials composed solely of SWNTs. Here we show that SWNTs dissolve at high concentration in acids; the SWNTs are stabilized because acids protonate their sidewalls, balancing wall-wall van der Waals forces. Acid strength controls the phase behaviour. At low concentration, SWNTs in acids dissolve as individual tubes which behave as Brownian rods. At higher concentration, SWNTs form a highly unusual nematic liquid phase consisting of spaghetti-like self assembled supermolecular strands of mobile, solvated tubes in equilibrium with a dilute isotropic phase. At even higher concentration, the spaghetti strands self-assemble into a polydomain nematic liquid crystal, where the domains are entangled with each other. Under anhydrous condition, the liquid crystalline phase can be processed into continuous highly aligned fibers of pure SWNTs without the aid of surfactants or polymers. By using a new fluorescent staining technique, we measure the rotational diffusivity and persistence length of SWNTs suspended in water with the aid of surfactants, and show that SWNTs behave as Brownian rods.

  15. Uptake of HCl and HOCl onto sulfuric acid. Solubilities, diffusivities, and reaction

    SciTech Connect

    Hanson, D.R.; Ravishankara, A.R. Univ. of Colorado, Boulder, CO )

    1993-11-25

    The interaction of HOCl and HCl vapors with liquid sulfuric acid surfaces was studied in a flow tube equipped with chemical ionization mass spectrometry detection. Time-dependent uptake of HCl and HOCl was measured. A methodology for deriving the value of the quantity H[radical]D[sub 1], (the product of the Henry's law coefficient and the square root of the liquid-phase diffusion coefficient) is discussed. The partial pressures of HCl over HCl-doped sulfuric acid solutions were also measured to directly determine H for HCl (H[sub HCl]*). Using the measured values of H[sub HCl]* and H[sub HCl]*[radical]D[sub 1], the value of D[sub 1] for HCl in 50 wt % sulfuric acid was extracted. Values for H[sub HOCl] and for the second-order rate coefficient for the reaction between dissolved HOCl and HCl were also obtained. The application of these results to modeling stratospheric heterogeneous processes in sulfuric acid aerosols is discussed. 31 refs., 14 refs., 3 tabs.

  16. Multifunctional water-soluble molecular capsules based on p-phosphonic acid calix[5]arene.

    PubMed

    Martin, Adam D; Boulos, Ramiz A; Hubble, Lee J; Hartlieb, Karel J; Raston, Colin L

    2011-07-14

    p-Phosphonic acid calix[5]arene forms molecular capsules in water based on two of the molecules, which can be loaded with carboplatin using intense shearing, and attached to single wall carbon nano-tubes. Spin coating of the capsules onto a substrate affords 2 nm fibres of stacked calixarenes, with the self-assembly understood using molecular modelling. PMID:21637889

  17. Comparative study of emulsifying properties in acidic condition of soluble polysaccharides fractions obtained from soy hull and defatted soy flour.

    PubMed

    Porfiri, María Cecilia; Cabezas, Darío Marcelino; Wagner, Jorge Ricardo

    2016-02-01

    The present study compares the emulsifying properties in acidic conditions of hull soluble polysaccharides (HSPS), soybean soluble polysaccharides (SSPS) and its mixtures. These fractions were obtained from byproducts of soybean processing industry (soy hull and residual fiber after isolation of soy cotyledon protein, respectively). Although SSPS is already characterized, HSPS is a novel fraction which has not been studied in deep and it is still unexplored as emulsifier. Dispersions of both fraction and a mixture 50:50 of them at pH 3.0 were used as aqueous phase (1.0-3.0 % w/w) in coarse and fine oil-in-water emulsions (oil mass fraction = 0.3). Its stability was evaluated through the evolution of backscattering profiles (%BS), particle size distribution and mean particle diameters. The rheology of the emulsions was also analyzed. Both fractions provided stability to creaming when increasing the polysaccharide concentration and energy of homogenization. While coarse emulsions were unstable systems, fine emulsions were stable enough and allowed a deeper analysis of the destabilizing processes. A bridging flocculation phenomenon in the presence of HSPS and HSPS/SSPS mixtures is suggested, which influences the creaming and rheological behavior. Also, coalescence index increases according HSPS and HSPS/SSPS concentrations, but particle sizes reached were smaller than in SSPS emulsions. Fine emulsions with 3 % of HSPS/SSPS mixtures yielded the best results on the overall stability at 28 days. So, functional properties of the fractions may improve by the formulation of emulsions consisting in mixtures of them. These results are of interest to the manufacturing of acidic foods, taking advantage of obtaining byproducts from residual materials. PMID:27162375

  18. Activation of Carbonyl-Containing Molecules with Solid Lewis Acids in Aqueous Media

    SciTech Connect

    Román-Leshkov, Yuriy; Davis, Mark E.

    2011-09-28

    Current interest in reacting carbonyl-containing molecules in aqueous media is primarily due to the growing emphasis on conversion of biomass to fuels and chemicals. Recently, solid Lewis acids have been shown to perform catalytic reactions with carbonyl-containing molecules such as sugars in aqueous media. Here, catalysis mediated by Lewis acids is briefly discussed, Lewis acid solids that perform catalysis in aqueous media are then described, and the review is concluded with a few comments on the outlook for the future.

  19. Interaction of water-soluble amino acid Schiff base complexes with bovine serum albumin: fluorescence and circular dichroism studies.

    PubMed

    Gharagozlou, Mehrnaz; Boghaei, Davar M

    2008-12-15

    Fluorescence spectroscopy in combination with circular dichroism (CD) spectroscopy were used to investigate the interaction of water-soluble amino acid Schiff base complexes, [Zn(L1,2)(phen)] where phen is 1,10-phenanthroline and H2L1,2 is amino acid Schiff base ligands, with bovine serum albumin (BSA) under the physiological conditions in phosphate buffer solution adjusted to pH 7.0. The quenching mechanism of fluorescence was suggested as static quenching according to the Stern-Volmer equation. Quenching constants were determined using the Stern-Volmer equation to provide a measure of the binding affinity between amino acid Schiff base complexes and BSA. The thermodynamic parameters DeltaG, DeltaH and DeltaS at different temperatures (298, 310 and 318K) were calculated. The results indicate that the hydrophobic and hydrogen bonding interactions play a major role in [Zn(L1)(phen)]-BSA association, whereas hydrophobic and electrostatic interactions participate a main role in [Zn(L2)(phen)]-BSA binding process. Binding studies concerning the number of binding sites and apparent binding constant Kb were performed by fluorescence quenching method. The distance R between the donor (BSA) and acceptor (amino acid Schiff base complexes) has been obtained utilizing fluorescence resonant energy transfer (FRET). Furthermore, CD spectra were used to investigate the structural changes of the BSA molecule with the addition of amino acid Schiff base complexes. The results indicate that the interaction of amino acid Schiff base complexes with BSA leads to changes in the secondary structure of the protein. Fractional contents of the secondary structure of BSA (f(alpha), f(beta), f(turn) and f(random)) were calculated with and without amino acid Schiff base complexes utilizing circular dichroism spectroscopy. Our results clarified that amino acid Schiff base complexes could bind to BSA and be effectively transported and eliminated in the body, which could be a useful guideline for

  20. Esterification of acidic oils over a versatile amorphous solid catalyst.

    PubMed

    Zaccheria, Federica; Brini, Simona; Psaro, Rinaldo; Scotti, Nicola; Ravasio, Nicoletta

    2009-01-01

    An amorphous SiO(2)-ZrO(2) catalyst shows high activity in the esterification of free fatty acids contained in vegetable oils while at the same time promoting the transesterification of triglycerides. The catalyst is hence a good candidate for a low-waste deacidification pretreatment or for a one-pot biodiesel production process starting from oils with a high acid content. PMID:19479893

  1. Sodium alginate as a potential carrier in solid dispersion formulations to enhance dissolution rate and apparent water solubility of BCS II drugs.

    PubMed

    Borba, Paola Aline Amarante; Pinotti, Marihá; de Campos, Carlos Eduardo Maduro; Pezzini, Bianca Ramos; Stulzer, Hellen Karine

    2016-02-10

    The solid dispersion technique is the most effective method for improving the dissolution rate of poorly water-soluble drugs, however it depends on a suitable carrier selection. The work explored the use of the biopolymer sodium alginate (SA) as a potential carrier in solid dispersions (SD). The data demonstrated that SA was able to improve the biopharmaceutical properties of the BCS II drug telmisartan (TEL) of low solubility even using relative small drug:polymer ratio. A solid state grinding process was used to prepare the solid dispersions (SD) during 45 min. The SD were prepared in different proportions of drug and carrier of 1:1, 1:3, 1:5, 1:7 and 1:9 (mass/mass). DSC, XRPD, FTIR and Raman confirmed the presence of molecular interactions between TEL and the carrier. FTIR supports the presence of hydrogen bonds between TEL and the carrier. SD_1:5, SD_1:7 and SD_1:9 enhanced the dissolution rate of the drug releasing more than 80% of the drug in just 30 min (83%, 84% and 87%). The the t-test results demonstrated equal dissolution efficiency values for SD_1:7 and Micardis(®), however the similarity (f2) and difference (f1) fit factors showed that the SD and Micardis(®) are statistically different. The physical stability studies demonstrated that SD using sodium alginate as a carrier remained unchanged during the period of 90 days at room temperature, showing that the sodium alginate acts as a good anti plasticizer agent, preventing the drug recrystallization. PMID:26686139

  2. Novel in situ self-assembly nanoparticles for formulating a poorly water-soluble drug in oral solid granules, improving stability, palatability, and bioavailability

    PubMed Central

    Guo, Shujie; Pham, Kevin; Li, Diana; Penzak, Scott R; Dong, Xiaowei

    2016-01-01

    Purpose The purpose of this study was to develop a novel lipid-based nanotechnology to formulate poorly water-soluble drugs in oral solid granules to improve stability, palatability, and bioavailability. Materials and methods In one method, we prepared ritonavir (RTV) nanoparticles (NPs) by a microemulsion-precursor method and then converted the RTV NPs to solid granules by wet granulation to produce RTV NP-containing granules. In the other innovative method, we did not use water in the formulation preparation, and discovered novel in situ self-assembly nanoparticles (ISNPs). We prepared RTV ISNP granules that did not initially contain NPs, but spontaneously produced RTV ISNPs when the granules were introduced to water with gentle agitation. We fully characterized these RTV nanoformulations. We also used rats to test the bioavailability of RTV ISNP granules. Finally, an Astree electronic tongue was used to assess the taste of the RTV ISNP granules. Results RTV NP-containing granules only had about 1% drug loading of RTV in the solid granules. In contrast, RTV ISNP granules achieved over 16% drug loading and were stable at room temperature over 24 weeks. RTV ISNPs had particle size between 160 nm and 300 nm with narrow size distribution. RTV ISNPs were stable in simulated gastric fluid for 2 hours and in simulated intestinal fluid for another 6 hours. The data from the electronic tongue showed that the RTV ISNP granules were similar in taste to blank ISNP granules, but were much different from RTV solution. RTV ISNP granules increased RTV bioavailability over 2.5-fold compared to RTV solution. Conclusion We successfully discovered and developed novel ISNPs to manufacture RTV ISNP granules that were reconstitutable, stable, and palatable, and improved RTV bioavailability. The novel ISNP nanotechnology is a platform to manufacture oral solid dosage forms for poorly water-soluble drugs, especially for pediatric formulation development. PMID:27103803

  3. MOF-Derived Tungstated Zirconia as Strong Solid Acids toward High Catalytic Performance for Acetalization.

    PubMed

    Wang, Peng; Feng, Jian; Zhao, Yupei; Wang, Shaobin; Liu, Jian

    2016-09-14

    A strong solid acid, tungstated zirconia (WZ), has been prepared first using tungstate immobilized UiO-66 as precursors through a "double-solvent" impregnation method under mild calcination temperature. With moderate W contents, the as-synthesized WZ catalysts possess a high density of acid sites, and the proper heat treatment also has facilely led to a bunch of oligomeric tungsten clusters on stabilized tetragonal ZrO2. The resultant solid acids show an improved catalytic performance toward the benzaldehyde's acetalization in comparison with traditional zirconium hydroxide-prepared WZ. Notably, due to large surface area and additionally introduced strong acid sites, the MOF-derived WZ catalysts afforded conversion up to 86.0%. The facile method endows the WZ catalysts with superior catalytic activities and excellent recyclability, thus opening a new avenue for preparation of metal oxide-based solid superacids and superbases. PMID:27557351

  4. Biosynthesis of Fatty Acids by a Soluble Extract From Developing Soybean Cotyledons 1

    PubMed Central

    Rinne, R. W.

    1969-01-01

    Fractionation of developing soybean cotyledons into cellular components demonstrates that most of the activity necessary to incorporate acetate-1-14C into lipid remains in the supernatant from a 198,000g spin for 1 hr. The system studied is dependent upon ATP, CoA, and CO2. Concentrations of ATP greater than 4 × 10−3m are inhibitory, while 1 × 10−4m CoA is needed for optimal activity. Avidin inhibition of acetate incorporation into lipid could be reversed by biotin. Studies indicated that NADPH is a better source of reducing power than NADH. The system studied is inhibited by p-chloromercuribenzoic acid and this inhibition can be reversed by an excess of GSH. The system studied shows maximum activity in tris buffer at pH 8.6 or in glycine buffer, pH 9.4. The distribution of acetate into the various fatty acids is greatly influenced by the temperature of incubation. Cooler incubation temperatures favor the distribution of acetate into the more unsaturated fatty acids. PMID:16657038

  5. Influence of solid-state acidity on the decomposition of sucrose in amorphous systems. I.

    PubMed

    Alkhamis, Khouloud A

    2008-10-01

    It was of interest to develop a method for solid-state acidity measurements using pH indicators and to correlate this method to the degradation rate of sucrose. Amorphous samples containing lactose 100mg/ml, sucrose 10mg/ml, citrate buffer (1-50mM) and sodium chloride (to adjust the ionic strength) were prepared by freeze-drying. The lyophiles were characterized using powder X-ray diffraction, differential scanning calorimetry and Karl Fischer titremetry. The solid-state acidity of all lyophiles was measured using diffuse reflectance spectroscopy and suitable indicators (thymol blue or bromophenol blue). The prepared lyophiles were subjected to a temperature of 60 degrees C and were analyzed for degradation using the Trinder kit. The results obtained from this study have shown that the solid-state acidity depends mainly on the molar ratio of the salt and the acid used in buffer preparation and not on the initial pH of the solution. The degradation of sucrose in the lyophiles is extremely sensitive to the solid-state acidity and the ionic strength. Reasonable correlation was obtained between the Hammett acidity function and sucrose degradation rate. The use of cosolvents (in the calibration plots) can provide good correlations with the rate of an acid-catalyzed reaction, sucrose inversion, in amorphous lyophiles. PMID:18647642

  6. Impact of Dry Solids and Bile Acid Concentrations on Bile Acid Binding Capacity of Extruded Oat Cereals

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Extruded breakfast cereals (EBC), processed from two oat lines, N979-5-2-4 (N979) and ‘Jim’, with beta-glucan concentrations of 8.7 and 4.9%, respectively, were used to determine the impact of dry solids (DS) and bile acid (BA) concentrations on in vitro BA binding efficiency. A full fractional fact...

  7. What Variables Affect Solubility?

    ERIC Educational Resources Information Center

    Baker, William P.; Leyva, Kathryn

    2003-01-01

    Helps middle school students understand the concept of solubility through hands-on experience with a variety of liquids and solids. As they explore factors that affect solubility and saturation, students gain content mastery and an understanding of the inquiry process. Also enables teachers to authentically assess student performance on several…

  8. Cloning and nucleotide sequencing of genes for three small, acid-soluble proteins from Bacillus subtilis spores.

    PubMed Central

    Connors, M J; Mason, J M; Setlow, P

    1986-01-01

    Three Bacillus subtilis genes (termed sspA, sspB, and sspD) which code for small, acid-soluble spore proteins (SASPs) have been cloned, and their complete nucleotide sequence has been determined. The amino acid sequences of the SASPs coded for by these genes are similar to each other and to those of the SASP-1 of B. subtilis (coded for by the sspC gene) and the SASP-A/C family of B. megaterium. The sspA and sspB genes are expressed only in sporulation, in parallel with each other and with the sspC gene. Two regions upstream of the postulated transcription start sites for the sspA and B genes have significant homology with the analogous regions of the sspC gene and the SASP-A/C gene family. Purification of two of the three major B, subtilis SASPs (alpha and beta) and determination of their amino-terminal sequences indicated that the sspA gene codes for SASP-alpha and that the sspB gene codes for SASP-beta. This was confirmed by the introduction of deletion mutations into the cloned sspA and sspB genes and transfer of these deletions into the B. subtilis chromosome with concomitant loss of the wild-type gene. Images PMID:3009398

  9. n-hydrocarbons conversions over metal-modified solid acid catalysts

    NASA Astrophysics Data System (ADS)

    Zarubica, A.; Ranđelović, M.; Momčilović, M.; Radulović, N.; Putanov, P.

    2013-12-01

    The quality of a straight-run fuel oil can be improved if saturated n-hydrocarbons of low octane number are converted to their branched counterparts. Poor reactivity of traditional catalysts in isomerization reactions imposed the need for the development of new catalysts among which noble metal promoted acid catalysts, liquid and/or solid acid catalysts take a prominent place. Sulfated zirconia and metal promoted sulfated zirconia exhibit high activity for the isomerization of light alkanes at low temperatures. The present paper highlights the original results which indicate that the modification of sulfated zirconia by incorporation of metals (platinum and rhenium) significantly affects catalytic performances in n-hydrocarbon conversion reactions. Favourable activity/selectivity of the promoted sulfated zirconia depends on the crystal phase composition, critical crystallites sizes, platinum dispersion, total acidity and type of acidity. Attention is also paid to the recently developed solid acid catalysts used in other conversion reactions of hydrocarbons.

  10. Synthesis and Anchoring of Antineoplastic Ferrocene and Phthalocyanine Derivatives on Water-Soluble Polymeric Drug Carriers Derived from Lysine and Aspartic Acid

    PubMed Central

    Maree, M. David; Neuse, Eberhard W.; Erasmus, Elizabeth; Swarts, Jannie C.

    2008-01-01

    The general synthetic strategy towards water-soluble biodegradable drug carriers and the properties that they must have are discussed. The syntheses of water-soluble biodegradable copolymers of lysine and aspartic acid as potential drug-delivering devices, having amine-functionalised side chains are then described. Covalent anchoring of carboxylic acid derivatives of the antineoplastic ferrocene and photodynamically active phthalocyanine moieties to the amine-containing drug carrier copolymers under mild coupling conditions has been achieved utilising the coupling reagent O-benzotriazolyl-N,N,N′,N′-tetramethyluronium hexafluorophosphate to promote formation of the biodegradable amide bond. Even though the parent antineoplastic ferrocene and phthalocyanine derivatives are themselves insoluble in water at pH < 7, the new carrier-drug conjugates that were obtained are well water-soluble. PMID:18288243

  11. Release of Water Soluble Drugs from Dynamically Swelling POLY(2-HYDROXYETHYL Methacrylate - CO - Methacrylic Acid) Hydrogels.

    NASA Astrophysics Data System (ADS)

    Kou, Jim Hwai-Cher

    In this study, ionizable copolymers of HEMA and methacrylic acid (MA) are investigated for their potential use in developing pH dependent oral delivery systems. Because of the MA units, these gels swell extensively at high pH. Since solute diffusion in the hydrophilic polymers depends highly on the water content of the matrix, it is anticipated that the release rate will be modulated by this pH induced swelling. From a practical point of view, the advantage of the present system is that one can minimize drug loss in the stomach and achieve a programmed release in intestine. This approach is expected to improve delivery of acid labile drugs or drugs that cause severe gastrointestinal side effects. This work mainly focuses on the basic understanding of the mechanism involved in drug release from the poly(HEMA -co- MA) gels, especially under dynamic swelling conditions. Equilibrium swelling is first characterized since water content is the major determinant of transport properties in these gels. Phenylpropanolamine (PPA) is chosen as the model drug for the release study and its diffusion characteristics in the gel matrix determined. The data obtained show that the PPA diffusivity follows the free volume theory of Yasuda, which explains the accelerating effect of swelling on drug release. A mathematical model based on a diffusion mechanism has been developed to describe PPA release from the swelling gels. Based on this model, several significant conclusions can be drawn. First, the release rate can be modulated by the aspect ratio of the cylindrical geometry, and this has a practical implication in dosage form design. Second, the release rate can be lowered quite considerably if the dimensional increase due to swelling is significant. Consequently, it is the balance between the drug diffusivity increase and the gel dimensional growth that determines the release rate from the swelling matrix. Third, quasi-steady release kinetics, which are characteristic of swelling

  12. Solid Dose Form of Metformin with Ethyl Eicosapentaenoic Acid Does Not Improve Metformin Plasma Availability

    PubMed Central

    Burton, Jeffrey H.; Johnson, William D.; Greenway, Frank L.

    2016-01-01

    Background The purpose of the study was to investigate effects of ethyl eicosapentaenoic acid on pharmacokinetics of metformin. Pharmacokinetic profiles of metformin and ethyl eicosapentaenoic acid when delivered separately or together in solid dose form were investigated and compared to determine whether the solid dose resulted in an altered metforminpharmacokinetics when given with or without food. Methods A single-center, open-label, repeated dose study investigated the pharmacokinetic (PK) profile of metformin when administered in solid dose form with ethyl eicosapentaenoic acid compared to co-administration with icosapent ethyl, an ester of eicosapentaenoic acid and ethyl alcohol used to treat severe hypertriglyceridemia with metformin hydrochloride. Non-compartmental PK methods were used to compare area under the plasma concentration curve (AUC) and maximum plasma concentration (Cmax) between patients randomized to either the ester or separate medications group under both fasting and fed conditions. Results Using these two PK parameters, results showed that metformin availability was higher under fasting conditions when delivered separately from icosapent ethyl. There were no group differences in the fed condition. Conclusions The solid dose form of metformin and ethyl eicosapentaenoic acid did not improve the pharmacokinetics of metformin in terms of plasma availability, suggesting that little is to be gained over the separate administration of ethyl eicosapentaenoic acid and metformin hydrochloride. PMID:26893954

  13. Effect of initial total solids concentration on volatile fatty acid production from food waste during anaerobic acidification.

    PubMed

    Wang, Quan; Jiang, Jianguo; Zhang, Yujing; Li, Kaimin

    2015-01-01

    The effect of initial total solids (TS) concentration on volatile fatty acid (VFAs) production from food waste under mesophilic conditions (35 °C) was determined. VFAs concentration and composition, biogas production, soluble chemical oxygen demand concentration, TS and volatile solids (VS) reduction, and ammonia nitrogen [Formula: see text] release were investigated. The VFAs concentrations were 26.10, 39.68, 59.58, and 62.64 g COD/L at TS contents of 40, 70, 100, and 130 g/L, respectively. While the VFAs' yields ranged from 0.467 to 0.799 g COD/g VSfed, decreased as initial TS increased. The percentage of propionate was not affected by TS concentration, accounting for 30.19-34.86% of the total VFAs, while a higher percentage of butyrate and lower percentage of acetate was achieved at a higher TS concentration. Biogas included mainly hydrogen and carbon dioxide and the maximum hydrogen yield of 148.9 ml/g VSfed was obtained at 130 g TS/L. [Formula: see text] concentration, TS and VS reductions increased as initial TS increased. Considering the above variables, we conclude that initial TS of 100 g/L shall be the most appropriate to VFAs production. PMID:25666310

  14. Amino acid digestibility of corn distillers dried grains with solubles, liquid condensed solubles, pulse dried thin stillage, and syrup balls fed to growing pigs.

    PubMed

    Soares, J A; Stein, H H; Singh, V; Shurson, G S; Pettigrew, J E

    2012-04-01

    Distillers dried grains with solubles (DDGS) has low and variable AA digestibility. The variability is often attributed to damage during the heating process, and it has been suggested that the damage happens to the soluble components of DDGS such as reducing sugars. Combining solubles and grains sometimes produces syrup balls (SB); their digestibility is unknown. The objective of this experiment was to identify potential sources of poor and variable AA digestibility in DDGS. Specifically, our objective was to determine whether the problems are associated with the solubles component or with SB. The ingredients evaluated were DDGS, intact SB, ground SB, liquid condensed solubles (LCS), and pulse dried thin stillage (PDTS) obtained from the same ethanol plant. The LCS is produced by evaporation of thin stillage. Each ingredient was used as the only source of AA in an experimental diet. In a duplicate 6 × 6 Latin square design with 7-d adaptation and collection periods, the 6 treatments consisted of an N-free diet and the 5 test ingredients. Pigs had 5 d of adaptation to each diet, and on d 6 and 7 ileal digesta were collected from an ileal cannula for 8 h each day. Both SB treatments had apparent ileal digestibility (AID) and standardized ileal digestibility (SID) of AA that were similar or greater (P < 0.05) than those of DDGS. The AID and SID values of Lys and a few other AA were similar in LCS (SID Lys: 63.1%) and DDGS (SID Lys: 61.5%), but the digestibility values of most AA in LCS were less than in DDGS (P < 0.05). The low digestibility of AA in LCS was most pronounced for Met (SID: LCS, 41.9% vs. DDGS, 82.8%). The LCS had less (P < 0.05) AID and SID of CP (SID: 67.8%) than intact SB (SID: 85.2%) and ground SB (SID: 85.9%) as well as all AA. The PDTS generally had the least AID and SID and had less (P < 0.05) CP (SID: 55.3%) and several AA, including Lys, compared with LCS. In conclusion, the presence of SB does not decrease AA digestibility of DDGS, and the LCS

  15. Species specific identification of spore-producing microbes using the gene sequence of small acid-soluble spore coat proteins for amplification based diagnostics

    DOEpatents

    McKinney, Nancy

    2002-01-01

    PCR (polymerase chain reaction) primers for the detection of certain Bacillus species, such as Bacillus anthracis. The primers specifically amplify only DNA found in the target species and can distinguish closely related species. Species-specific PCR primers for Bacillus anthracis, Bacillus globigii and Clostridium perfringens are disclosed. The primers are directed to unique sequences within sasp (small acid soluble protein) genes.

  16. [*C]octanoic acid breath test to measure gastric emptying rate of solids.

    PubMed

    Maes, B D; Ghoos, Y F; Rutgeerts, P J; Hiele, M I; Geypens, B; Vantrappen, G

    1994-12-01

    We have developed a breath test to measure solid gastric emptying using a standardized scrambled egg test meal (250 kcal) labeled with [14C]octanoic acid or [13C]octanoic acid. In vitro incubation studies showed that octanoic acid is a reliable marker of the solid phase. The breath test was validated in 36 subjects by simultaneous radioscintigraphic and breath test measurements. Nine healthy volunteers were studied after intravenous administration of 200 mg erythromycin and peroral administration of 30 mg propantheline, respectively. Erythromycin significantly enhanced gastric emptying, while propantheline significantly reduced gastric emptying rates. We conclude that the [*C]octanoic breath test is a promising and reliable test for measuring the gastric emptying rate of solids. PMID:7995200

  17. Rapid purification and direct microassay of calbindin9kDa utilizing its solubility in perchloric acid.

    PubMed Central

    Hubbard, M J

    1993-01-01

    The 9 kDa calcium-binding protein, calbindin9kDa, was found to be soluble in 7% (v/v) perchloric acid. Calbindin9kDa was easily purified from rat duodenum in 1 day with perchloric acid precipitation followed by reverse-phase h.p.l.c. The yield was 21.4 +/- 2.3 nmol/g wet weight of tissue (mean +/- S.E.M.; n = 3) from normally fed 7-8-week-old rats (approx. 70% recovery). The purification was also effective with rabbit duodenum calbindin9kDa, but not with various other EF-hand calcium-binding proteins tested in the rat. Several criteria (h.p.l.c., u.v. spectrum, denaturing two-dimensional PAGE, N-terminal sequencing) indicated that the rat calbindin9kDa was purified to homogeneity and was not affected by proteolysis. High-affinity calcium-binding properties were retained and no evidence of isoforms or charge modification was observed. Residue 59, identified as Asn (not Asp as previously reported), was fully amidated. When adopted as a microassay with isocratic h.p.l.c., the perchloric acid procedure enabled rapid (less than 6 min) and direct (peptide bond absorbance) quantification of less than 1 pmol of calbindin9kDa. This new approach to purification and assay will be of particular utility for investigations of calbindin9kDa in previously intractable low-abundance sources (e.g. cultured cells). Images Figure 1 Figure 2 PMID:8392333

  18. Use of hydrochloric acid for determinining solid-phase arsenic partitioning in sulfidic sediments.

    PubMed

    Wilkin, Richard T; Ford, Robert G

    2002-11-15

    We examined the use of room-temperature hydrochloric acid (1-6 M) and salt solutions of magnesium chloride, sodium carbonate, and sodium sulfide for the removal of arsenic from synthetic iron monosulfides and contaminated sediments containing acid-volatile sulfides (AVS). Results indicate that acid-soluble arsenic reacts with H2S released from AVS phases and precipitates at low pH as disordered orpiment or alacranite. Arsenic sulfide precipitation is consistent with geochemical modeling in that conditions during acid extraction are predicted to be oversaturated with respect to orpiment, realgar, or both. Binding of arsenic with sulfide at low pH is sufficiently strong that 6 M HCl will not keep spiked arsenic in the dissolved fraction. Over a wide range of AVS concentrations and molar [As]/[AVS] ratios, acid extraction of arsenic from sulfide-bearing sediments will give biased results that overestimate the stability or underestimate the bioavailability of sediment-bound arsenic. Alkaline solutions of sodium sulfide and sodium carbonate are efficient in removing arsenic from arsenic sulfides and mixed iron-arsenic sulfides because of the high solubility of arsenic at alkaline pH, the formation of stable arsenic complexes with sulfide or carbonate, or both. PMID:12487318

  19. Chemical modeling of acid-base properties of soluble biopolymers derived from municipal waste treatment materials.

    PubMed

    Tabasso, Silvia; Berto, Silvia; Rosato, Roberta; Marinos, Janeth Alicia Tafur; Ginepro, Marco; Zelano, Vincenzo; Daniele, Pier Giuseppe; Montoneri, Enzo

    2015-01-01

    This work reports a study of the proton-binding capacity of biopolymers obtained from different materials supplied by a municipal biowaste treatment plant located in Northern Italy. One material was the anaerobic fermentation digestate of the urban wastes organic humid fraction. The others were the compost of home and public gardening residues and the compost of the mix of the above residues, digestate and sewage sludge. These materials were hydrolyzed under alkaline conditions to yield the biopolymers by saponification. The biopolymers were characterized by 13C NMR spectroscopy, elemental analysis and potentiometric titration. The titration data were elaborated to attain chemical models for interpretation of the proton-binding capacity of the biopolymers obtaining the acidic sites concentrations and their protonation constants. The results obtained with the models and by NMR spectroscopy were elaborated together in order to better characterize the nature of the macromolecules. The chemical nature of the biopolymers was found dependent upon the nature of the sourcing materials. PMID:25658795

  20. Near-Infrared Electrogenerated Chemiluminescence from Aqueous Soluble Lipoic Acid Au Nanoclusters.

    PubMed

    Wang, Tanyu; Wang, Dengchao; Padelford, Jonathan W; Jiang, Jie; Wang, Gangli

    2016-05-25

    Strong electrogenerated chemiluminescence (ECL) is detected from dithiolate Au nanoclusters (AuNCs) in aqueous solution under ambient conditions. A novel mechanism to drastically enhance the ECL is established by covalent attachment of coreactants N,N-diethylethylenediamine (DEDA) onto lipoic acid stabilized Au (Au-LA) clusters with matching redox activities. The materials design reduces the complication of mass transport between the reactants during the lifetime of radical intermediates involved in conventional ECL generation pathway. The intracluster reactions are highly advantageous for applications by eliminating additional and high excess coreactants otherwise needed. The enhanced ECL efficiency also benefits uniquely from the multiple energy states per Au cluster and multiple DEDA ligands in the monolayer. Potential step and sweeping experiments reveal an onset potential of 0.78 V for oxidative-reduction ECL generation. Multifolds higher efficiency is found for the Au clusters alone in reference to the standard Rubpy with high excess TPrA. The ECL in near-IR region (beyond 700 nm) is highly advantageous with drastically reduced interference signals over visible ones. The features of ECL intensity responsive to electrode potential and solution pH under ambient conditions make Au-LA-DEDA clusters promising ECL reagents for broad applications. The strategy to attach coreactants on Au clusters is generalizable for other nanomaterials. PMID:27172252

  1. Chemical Modeling of Acid-Base Properties of Soluble Biopolymers Derived from Municipal Waste Treatment Materials

    PubMed Central

    Tabasso, Silvia; Berto, Silvia; Rosato, Roberta; Tafur Marinos, Janeth Alicia; Ginepro, Marco; Zelano, Vincenzo; Daniele, Pier Giuseppe; Montoneri, Enzo

    2015-01-01

    This work reports a study of the proton-binding capacity of biopolymers obtained from different materials supplied by a municipal biowaste treatment plant located in Northern Italy. One material was the anaerobic fermentation digestate of the urban wastes organic humid fraction. The others were the compost of home and public gardening residues and the compost of the mix of the above residues, digestate and sewage sludge. These materials were hydrolyzed under alkaline conditions to yield the biopolymers by saponification. The biopolymers were characterized by 13C NMR spectroscopy, elemental analysis and potentiometric titration. The titration data were elaborated to attain chemical models for interpretation of the proton-binding capacity of the biopolymers obtaining the acidic sites concentrations and their protonation constants. The results obtained with the models and by NMR spectroscopy were elaborated together in order to better characterize the nature of the macromolecules. The chemical nature of the biopolymers was found dependent upon the nature of the sourcing materials. PMID:25658795

  2. Thermodynamics of aragonite-strontianite solid solutions: Results from stoichiometric solubility at 25 and 76°C

    USGS Publications Warehouse

    Plummer, L.N.; Busenberg, E.

    1987-01-01

    Neither equilibrium nor stoichiometric saturation is observed at 76°C during laboratory recrystallization of strontianite-aragonite solid solutions even after apparent 100 percent conversion to a narrow secondary composition and demonstration of a nearly constant composition system for periods of 300 hours.

  3. A new synthetic methodology for the preparation of biocompatible and organo-soluble barbituric- and thiobarbituric acid based chitosan derivatives for biomedical applications.

    PubMed

    Shahzad, Sohail; Shahzadi, Lubna; Mahmood, Nasir; Siddiqi, Saadat Anwar; Rauf, Abdul; Manzoor, Faisal; Chaudhry, Aqif Anwar; Rehman, Ihtesham Ur; Yar, Muhammad

    2016-09-01

    Chitosan's poor solubility especially in organic solvents limits its use with other organo-soluble polymers; however such combinations are highly required to tailor their properties for specific biomedical applications. This paper describes the development of a new synthetic methodology for the synthesis of organo-soluble chitosan derivatives. These derivatives were synthesized from chitosan (CS), triethyl orthoformate and barbituric or thiobarbituric acid in the presence of 2-butannol. The chemical interactions and new functional motifs in the synthesized CS derivatives were evaluated by FTIR, DSC/TGA, UV/VIS, XRD and (1)H NMR spectroscopy. A cytotoxicity investigation for these materials was performed by cell culture method using VERO cell line and all the synthesized derivatives were found to be non-toxic. The solubility analysis showed that these derivatives were readily soluble in organic solvents including DMSO and DMF. Their potential to use with organo-soluble commercially available polymers was exploited by electrospinning; the synthesized derivatives in combination with polycaprolactone delivered nanofibrous membranes. PMID:27207049

  4. Molecularly imprinted polymer microspheres for solid-phase extraction of protocatechuic acid in Rhizoma homalomenae.

    PubMed

    Chen, Fang-Fang; Wang, Guo-Ying; Shi, Yan-Ping

    2011-10-01

    Molecularly imprinted polymers (MIPs) had been prepared by precipitation polymerization method using acrylamide as the functional monomer, ethylene glycol dimethacrylate as the cross-linker, acetonitrile as the porogen solvent and protocatechuic acid (PA), one of phenolic acids, as the template molecule. The MIPs were characterized by scanning electron microscopy and Fourier transform infrared, and their performance relative to non-imprinted polymers was assessed by equilibrium binding experiments. Six structurally similar phenolic acids, including p-hydroxybenzoic acid, gallic acid, salicylic acid, syringic acid, vanillic acid, ferulic acid were selected to assess the selectivity and recognition capability of the MIPs. The MIPs were applied to extract PA from the traditional Chinese medicines as a solid-phase extraction sorbent. The resultant cartridge showed that the MIPs have a good extraction performance and were able to selectively extract almost 82% of PA from the extract of Rhizoma homalomenae. Thus, the proposed molecularly imprinted-solid phase extraction-high performance liquid chromatography method can be successfully used to extract and analyse PA in traditional Chinese medicines. PMID:21809445

  5. Solid-State Forms of β-Resorcylic Acid: How Exhaustive Should a Polymorph Screen Be?

    PubMed Central

    2010-01-01

    A combined experimental and computational study was undertaken to establish the solid-state forms of β-resorcylic acid (2,4-dihydroxybenzoic acid). The experimental search resulted in nine crystalline forms: two concomitantly crystallizing polymorphs, five novel solvates (with acetic acid, dimethyl sulfoxide, 1,4-dioxane, and two with N,N-dimethyl formamide), in addition to the known hemihydrate and a new monohydrate. Form II°, the thermodynamically stable polymorph at room temperature, was found to be the dominant crystallization product. A new, enantiotropically related polymorph (form I) was obtained by desolvation of certain solvates, sublimation experiments, and via a thermally induced solid−solid transformation of form II° above 150 °C. To establish their structural features, interconversions, and relative stability, all solid-state forms were characterized with thermal, spectroscopic, X-ray crystallographic methods, and moisture-sorption analysis. The hemihydrate is very stable, while the five solvates and the monohydrate are rather unstable phases that occur as crystallization intermediates. Complementary computational work confirmed that the two experimentally observed β-resorcylic acid forms I and II° are the most probable polymorphs and supported the experimental evidence for form I being disordered in the p-OH proton position. These consistent outcomes suggest that the most practically important features of β-resorcylic acid crystallization under ambient conditions have been established; however, it appears impractical to guarantee that no additional metastable solid-state form could be found. PMID:21218174

  6. Bench-Scale and Pilot-Scale Treatment Technologies for the Removal of Total Dissolved Solids from Coal Mine Water: A Review

    EPA Science Inventory

    Coal mine water (CMW) is typically treated to remove suspended solids, acidity, and soluble metals, but high concentrations of total dissolved solids (TDS) have been reported to impact the environment at several CMW discharge points. Consequently, various states have establishe...

  7. Directed evolution and structural analysis of N-carbamoyl-D-amino acid amidohydrolase provide insights into recombinant protein solubility in Escherichia coli

    SciTech Connect

    Jiang, Shimin; Li, Chunhong; Zhang, Weiwen; Cai, Yuanheng; Yang, Yunlin; Yang, Sheng; Jiang, Weihong

    2007-03-15

    One of the greatest bottlenecks in producing recombinant proteins in Escherichia coli is that over-expressed target proteins are mostly present in an insoluble form without any biological activity. N-carbamoyl-D-amino-acid amidohydrolase (DCase) is an important enzyme involved in semi-synthesis of β-lactam antibiotics in industry. In this study, in order to determine the amino acid sites responsible for solubility in DCase, error-prone PCR and DNA shuffling techniques are applied to randomly mutate its encoding sequence, followed by an efficient screening based on structural complementation. Several mutants of DCase with reduced aggregation are isolated. Solubility tests of these mutants and several other mutants generated by site-directed mutagenesis indicate that three amino acid residues of DCase (A18, Y30 and K34) are related to the protein solubility in DCase. In silico structural modeling analyses further suggest that hydrophilicity and/or negative charge at these three residues may be responsible for the increased solubility of DCase proteins in E. coli. Based on the information, multiple engineering designated mutants were constructed by site-directed mutagenesis; among them, a triple mutant A18T/Y30N/K34E (named as DCase-M3) can be over-expressed in E. coli with up to 80% of DCase-M3 protein as soluble. DCase-M3 is purified to homogeneity and a comparative analysis with WT DCase demonstrates that DCase-M3 enzyme is similar to the native DCase in terms of its kinetic and thermodynamic properties. The study provides new insights on recombinant protein solubility in E. coli.

  8. On the acidity of saponite materials: a combined HRTEM, FTIR, and solid-state NMR study.

    PubMed

    Bisio, C; Gatti, G; Boccaleri, E; Marchese, L; Bertinetti, L; Coluccia, S

    2008-03-18

    Acid clays were prepared by exchanging a synthetic saponite in HCl solutions of different concentration (0.01 and 1M, respectively). A combined experimental approach (XRD, HRTEM, N2 physisorption, solid-state MAS NMR, and TGA) was used to investigate on the structural, morphological, and textural features of the samples treated under mild and strong acid conditions. FTIR spectroscopy of adsorbed probe molecules with different basicity (e.g., CO and NH3) was used to monitor the surface acid properties and acid site distribution. XRD and SS-MAS NMR indicated that the activation under mild acid conditions does not alter the clay structure, while a deep modification of the saponite framework occurred after ion exchange in 1 M HCl solution. The presence of porous amorphous silica phase after treatment under strong acid conditions was confirmed by TEM inspection augmented by SS-MAS NMR and FTIR spectroscopy. N2 and Ar physisorption measurements suggested that cavitation phenomena occurred in saponite structure. N2 physisorption confirmed that the porosity and surface area of the samples are strongly modified upon strong acid treatment. FTIR spectroscopy of adsorbed NH3 pointed out that the H-exchange in mild conditions increased the number of surface Brønsted acid sites. Conversely, these sites are significantly depleted after treatment under strong acid conditions. The use of CO as a FTIR probe molecule, which is applied for the first time to study synthetic acid clays, allowed to monitor distribution and strength of Brønsted acid sites, whose acidity is similar to that of strong acid zeolites. The Al-OH sites with medium acidity are also found in acid-activated saponites. The distribution of strong and medium acid sites is strictly dependent on the acid conditions adopted. PMID:18251562

  9. Prevention of DNA damage in spores and in vitro by small, acid-soluble proteins from Bacillus species.

    PubMed Central

    Fairhead, H; Setlow, B; Setlow, P

    1993-01-01

    The DNA in dormant spores of Bacillus species is saturated with a group of nonspecific DNA-binding proteins, termed alpha/beta-type small, acid-soluble spore proteins (SASP). These proteins alter DNA structure in vivo and in vitro, providing spore resistance to UV light. In addition, heat treatments (e.g., 85 degrees C for 30 min) which give little killing of wild-type spores of B. subtilis kill > 99% of spores which lack most alpha/beta-type SASP (termed alpha - beta - spores). Similar large differences in survival of wild-type and alpha - beta - spores were found at 90, 80, 65, 22, and 10 degrees C. After heat treatment (85 degrees C for 30 min) or prolonged storage (22 degrees C for 6 months) that gave > 99% killing of alpha - beta - spores, 10 to 20% of the survivors contained auxotrophic or asporogenous mutations. However, alpha - beta - spores heated for 30 min at 85 degrees C released no more dipicolinic acid than similarly heated wild-type spores (< 20% of the total dipicolinic acid) and triggered germination normally. In contrast, after a heat treatment (93 degrees C for 30 min) that gave > or = 99% killing of wild-type spores, < 1% of the survivors had acquired new obvious mutations, > 85% of the spore's dipicolinic acid had been released, and < 1% of the surviving spores could initiate spore germination. Analysis of DNA extracted from heated (85 degrees C, 30 min) and unheated wild-type spores and unheated alpha - beta - spores revealed very few single-strand breaks (< 1 per 20 kb) in the DNA. In contrast, the DNA from heated alpha- beta- spores had more than 10 single-strand breaks per 20 kb. These data suggest that binding of alpha/beta-type SASP to spore DNA in vivo greatly reduces DNA damage caused by heating, increasing spore heat resistance and long-term survival. While the precise nature of the initial DNA damage after heating of alpha- beta- spores that results in the single-strand breaks is not clear, a likely possibility is DNA depurination. A

  10. An investigation of the applicability of attenuated total reflection infrared spectroscopy for measurement of solubility and supersaturation of aqueous citric acid solutions

    NASA Astrophysics Data System (ADS)

    Dunuwila, Dilum D.; Carroll, Leslie B.; Berglund, Kris A.

    1994-04-01

    Currently applied methods for measurement of solubility and supersaturation based on viscometry, refractometry, interferometry and density require the separation of phases prior to measurement. ATR (attenuated total reflection) infrared spectroscopy provides a unique configuration in which the infrared spectrum of a liquid phase can be obtained in a slurry without phase separation. The applicability of the technique was investigated using a micro Circle ® open boat cell equipped with a ZnSe (zinc selenide) ATR rod. Experiments conducted with aqueous citric acid proved that ATR infrared spectroscopy can be successfully employed to determine solubility and supersaturation.

  11. Role of solid acid catalysts in bio diesel production.

    PubMed

    Shivayogimath, C B; Sunita, G; Manoj Kumar, B

    2009-07-01

    Biodiesel is gaining importance as an alternate source of attractive fuel because of depleting fossil fuel resources. It is produced by trans-esterification, in which oil or fat reacts with a monohydric alcohol in presence of a catalyst. In the present work, trans-esterification of sunflower oil with methanol is carried out by using zirconia supported isopoly and heteropoly tungstates (HPAs) as catalysts. Effects of reaction parameters, such as catalyst types and its concentration, molar ratio of sunflower oil to methanol, reaction temperature and time, have been optimized to get higher conversion of sunflower oil and the product distribution of fatty acid methyl esters (FAME) in the trans-esterfication reaction. PMID:21117436

  12. Effervescence Assisted Fusion Technique to Enhance the Solubility of Drugs.

    PubMed

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

    2015-12-01

    The solubility of five poorly soluble drugs was enhanced by using an effervescence assisted solid dispersion (EASD) technique. EASDs were prepared by using modified fusion method. Drug and hydrophilic carrier were melted, and in this molten mixture, effervescence was generated by adding effervescence couple comprising organic acid (citric acid) and carbonic base (sodium bicarbonate). Solubility of drug powders, solid dispersions, and EASDs was determined at 25°C using shake flask method. Atorvastatin calcium, cefuroxime axetil, clotrimazole, ketoconazole, and metronidazole benzoate were estimated using a spectrophotometer at 246, 280, 260, 230, and 232 nm (λ max), respectively. Solubility of atorvastatin calcium (from 100 to 345 μg/ml), cefuroxime axetil (from 441 to 1948 μg/ml), clotrimazole (from 63 to 677 μg/ml), ketoconazole (from 16 to 500 μg/ml), and metronidazole benzoate (from 112 to 208 μg/ml) in EASDs was enhanced by 3.45-, 4.4-, 10.7-, 31.2-, and 1.8-fold, respectively. Scanning electron micrographs of drug powder, solid dispersion, and EASDs were compared. Scanning electron micrographs of EASDs showed a uniform distribution of drug particles in the carrier matrix. Morphology (size and shape) of cefuroxime axetil particles was altered in solid dispersion as well as in EASD. EASDs showed better solubility enhancement than conventional solid dispersions. The present technique is better suitable for drugs having a low melting point or melt without charring. Effervescence assisted fusion technique of preparing solid dispersions can be employed for enhancing solubility, dissolution, and bioavailability of poorly soluble drugs. PMID:26265190

  13. Sulfonated mesoporous silica-carbon composites and their use as solid acid catalysts

    NASA Astrophysics Data System (ADS)

    Valle-Vigón, Patricia; Sevilla, Marta; Fuertes, Antonio B.

    2012-11-01

    The synthesis of highly functionalized porous silica-carbon composites made up of sulfonic groups attached to a carbon layer coating the pores of three types of mesostructured silica (i.e. SBA-15, KIT-6 and mesocellular silica) is presented. The synthesis procedure involves the following steps: (a) removal of the surfactant, (b) impregnation of the silica pores with a carbon precursor, (c) carbonization and (d) sulfonation. The resulting silica-carbon composites contain ˜30 wt % of carbonaceous matter with a high density of acidic groups attached to the deposited carbon (i.e.sbnd SO3H, sbnd COOH and sbnd OH). The structural characteristics of the parent silica are retained in the composite materials, which exhibit a high surface area, a large pore volume and a well-ordered porosity made up uniform mesopores. The high density of the sulfonic groups in combination with the mesoporous structure of the composites ensures that a large number of active sites are easily accessible to reactants. These sulfonated silica-carbon composites behave as eco-friendly, active, selective, water tolerant and recyclable solid acids. In this study we demonstrate the usefulness of these composites as solid acid catalysts for the esterification of maleic anhydride, succinic acid and oleic acid with ethanol. These composites exhibit a superior intrinsic catalytic activity to other commercial solid acids such as Amberlyst-15.

  14. Acid-Soluble Internal Capsules for Closed-Face Cassette Elemental Sampling and Analysis of Workplace Air

    PubMed Central

    Harper, Martin; Ashley, Kevin

    2013-01-01

    Airborne particles that are collected using closed-face filter cassettes (CFCs), which are used widely in the sampling of workplace aerosols, can deposit in places other than on the filter and thereby may not be included in the ensuing analysis. A technique for ensuring that internal non-filter deposits are included in the analysis is to collect airborne particles within an acid-soluble internal capsule that, following sampling, can be dissolved along with the filter for subsequent elemental analysis. An interlaboratory study (ILS) was carried out to evaluate the use of cellulosic CFC capsule inserts for their suitability in the determination of trace elements in airborne samples. The ILS was performed in accordance with an applicable ASTM International standard practice, ASTM E691, which describes statistical procedures for investigating interlaboratory precision. Performance evaluation materials consisted of prototype cellulose acetate capsules attached to mixed-cellulose ester filters. Batches of capsules were dosed with Pb-containing materials (standard aqueous solutions, and certified reference material soil and paint). Also, aerosol samples containing nine target analyte elements (As, Cd, Co, Cr, Cu, Fe, Pb, Mn, and Ni) were generated using a multiport sampler; various concentrations and sampling times were employed to yield samples fortified at desired loading levels. Triplicates of spiked capsules at three different loadings were conveyed to each volunteer laboratory; loading levels were unknown to the participants. The laboratories were asked to prepare the samples by acid dissolution and to analyze aliquots of extracted samples by atomic spectrometry in accordance with applicable ASTM International Standards. Participants were asked to report their results in units of μg of each target element per sample. For the elements investigated, interlaboratory precision and recovery estimates from the participating laboratories demonstrated the utility of the

  15. Water-soluble N-[(2-hydroxy-3-trimethylammonium)propyl]chitosan chloride as a nucleic acids vector for cell transfection.

    PubMed

    Faizuloev, Evgeny; Marova, Anna; Nikonova, Alexandra; Volkova, Irina; Gorshkova, Marina; Izumrudov, Vladimir

    2012-08-01

    To endow the cationic polysaccharides with solubility in the whole pH-range without loss of functionality of the amino groups, different chitosan samples were treated with glycidyltrimethylammonium chloride. Each modified unit of the exhaustively alkylated quaternized chitosan (QCht) contained both quaternary and secondary amino groups. The intercalated dye displacement assay and ζ-potential measurements implied stability of QCht polyplexes at physiological conditions and protonation of the secondary amino groups in slightly acidic media which is favorable for transfection according to proton sponge mechanism. The cytotoxicity and transfection efficacy increased with the chain lengthening. Nevertheless, the longest chains of QCht, 250 kDa were less toxic than PEI for COS-1 cells and revealed comparable and even significantly higher transfection activity of siRNA and plasmid DNA, respectively. Thus, highly polymerized QCht (250 kDa) provided the highest level of the plasmid DNA transfection being 5 and 80 times more active than QCht (100 kDa) and QCht (50 kDa), respectively, and 4-fold more effective than PEI, 25 kDa. The established influence of QCht molecular weight on toxicity and transfection efficacy allows elaborating polysaccharide vectors that possess rational balance of these characteristics. PMID:24750918

  16. Effect of hydration temperature on the solubility behavior of Ca-, S-, Al-, and Si-bearing solid phases in Portland cement pastes

    SciTech Connect

    Thomas, Jeffrey J.; Rothstein, David; Jennings, Hamlin M.; Christensen, Bruce J

    2003-12-01

    The concentrations of Ca, S, Al, Si, Na, and K in the pore solutions of ordinary Portland cement and white Portland cement pastes were measured during the first 28 d of curing at temperatures ranging from 5-50 deg. C. Saturation indices with respect to solid phases known to form in cement paste were calculated from a thermodynamic analysis of the elemental concentrations. Calculated saturation levels in the two types of paste were similar. The solubility behavior of Portlandite and gypsum at all curing temperatures was in agreement with previously reported behavior near room temperature. Saturation levels of both ettringite and monosulfate decreased with increasing curing temperature. The saturation level of ettringite was greater than that of monosulfate at lower curing temperatures, but at higher temperatures there was effectively no difference. The solubility behavior of C-S-H gel was investigated by applying an appropriate ion activity product (IAP) to the data. The IAP{sub CSH} decreased gradually with hydration time, and at a given hydration time the IAP{sub CSH} was lower at higher curing temperatures.

  17. Solid state solubility of miconazole in poly[(ethylene glycol)-g-vinyl alcohol] using hot-melt extrusion.

    PubMed

    Litvinov, V M; Guns, S; Adriaensens, P; Scholtens, B J R; Quaedflieg, M P; Carleer, R; Van den Mooter, G

    2012-10-01

    The use of hot-melt extrusion for preparing homogeneous API-excipient mixtures is studied for miconazole-PEG-g-PVA [poly(ethylene glycol)-poly(vinyl alcohol) graft copolymer] solid dispersions with a 5 cm(3) table-top, twin-screw corotating microcompounder (DSM Xplore). Phase behavior of PEG-g-PVA, miscibility of miconazole in PEG-g-PVA and the partitioning of miconazole between PEG and PVA amorphous phases are characterized using a combination of modulated DSC, XRPD, and solid-state (1)H and (13)C NMR methods. The (1)H NMR transverse magnetization relaxation (T(2) relaxation) method is used to analyze the phase composition and molecular mobility of the copolymer. The T(2) relaxation decay of pure PEG-g-PVA can be described by four T(2) relaxation components in the temperature range studied. PVA crystallinity is not largely affected by hot-melt extrusion and the presence of the drug. Miconazole preferably resides in the PEG amorphous phase, and its molecules are well dispersed in the PEG-g-PVA matrix using hot-melt extrusion mixing. Miconazole forms amorphous nanoclusters whose average size equals approximately 1.6 nm, indicating solid solution formation (molecular level dispersion) of the drug in the polymer. PMID:22905779

  18. [Preparation of two poor water soluble drugs - nanoporous ZnO solid dispersions and the mechanism of drug dissolution improvement].

    PubMed

    Gao, Bei; Sun, Chang-shan; Zhi, Zhuang-zhi; Wang, Yan; Chang, Di; Wang, Si-ling; Jiang, Tong-ying

    2011-11-01

    Nanoporous ZnO was used as a carrier to prepare drug solid dispersion, the mechanism of which to improve the drug dissolution was also studied. Nanoporous ZnO, obtained through chemical deposition method, was used as a carrier to prepare indomethacin and cilostazol solid dispersions by melt-quenching method, separately. The results of scanning electron microscope, surface area analyzer, fourier transform infra-red spectroscopy, differential scanning calorimeter and X-ray diffraction showed that drugs were implanted into nanopores of ZnO by physical adsorption effect and highly dispersed into nanopores of ZnO in amorphous form, moreover, these nanopores strongly inhibited amorphous recrystallization in the condition of 45 degrees C and 75% RH. In addition, the results of the dissolution tested in vitro exhibited that the accumulated dissolutions of indomethacin and cilostazol solid dispersions achieved about 90% within 5 min and approximately 80% within 30 min. It was indicated in this study that the mechanism of drug dissolution improvement was associated with the effects of nanoporous ZnO carrier on increasing drug dispersion, controlling drug in nanopores as amorphous form and inhibiting amorphous recrystallization. PMID:22260037

  19. Continuous Isosorbide Production From Sorbitol Using Solid Acid Catalysis

    SciTech Connect

    Williamson, R.; Holladay,J.; Jaffe, M.; Brunelle, D.

    2006-09-29

    This is a final report for a project funded by the US Department of Agriculture and managed by the US Department of Energy. The Iowa Corn Promotion Board was the principal contracting entity for the grant. The Iowa Corn Promotion Board subcontracted with General Electric, Pacific Northwest National Lab and New Jersey Institute of Technology to conduct research in this project. The Iowa Corn Promotion Board and General Electric provided cost share for the project. The purpose of this diverse collaboration was to integrate both the conversion and the polymer applications into one project and increase the likelihood of success. This project has led to additional collaborations among other polymer companies. The goals of the project were to develop a renewable route to isosorbide for commercialization that is economically competitive with all existing production technologies and to develop new applications for isosorbide in various products such as polymers and materials. Under this program a novel process for the production of isosorbide was developed and evaluated. The novel process converts corn based sorbitol into isosorbide using a solid catalyst with integrated water removal and product recovery. In addition the work under this program has identified several novel products based on isosorbide chemistries. These market applications include: epoxy resins, UV stabilizers, plasticizers and polyesters. These market applications have commercial interest within the current polymer industry. This report contains an overview summary of the accomplishments. Six inventions and four patent applications have been written as a result of this project. Additional data will be published in the patent applications. The data developed at New Jersey Institute of Technology was presented at two technical conferences held in June of 2006. Several companies have made inquiries about using this material in their products.

  20. Solubility and dissolution enhancement of efavirenz hot melt extruded amorphous solid dispersions using combination of polymeric blends: A QbD approach.

    PubMed

    Pawar, Jaywant; Tayade, Apurva; Gangurde, Avinash; Moravkar, Kailas; Amin, Purnima

    2016-06-10

    Efavirenz is a non-nucleoside reverse transcriptase inhibitor and categorized in to BCS class II drug. The aim of the present investigation was to apply quality by design approach to enhance the solubility, dissolution and stability of amorphous solid dispersions (ASDs) of efavirenz using a combination of Soluplus® and HPMCAS-HF polymers. In design of experiments, the user defined quadratic model was used to study the effect of variable concentrations of Soluplus® and HPMCAS-HF for the formation of ASDs of efavirenz. Similarly, a prototype ASD was made using Soluplus® as a carrier with efavirenz loading of 30%. The efavirenz ASDs granular extrudates were evaluated for saturation solubility as well as dissolution rate studies. X-ray powder diffraction, Differential scanning calorimetry, Fourier transform infrared, Atomic force microscopy and FTIR imaging to determine the solid state of efavirenz in the ASDs. DSC and XRD data confirmed that bulk crystalline efavirenz transformed to the amorphous form during the hot melt extrusion processing. Prototype ASD batch showed instability upon storage as per ICH guidelines over a period of 6months, observations inferred from DSC, XRD and in vitro dissolution studies. The maximum dissolution rate was observed when Soluplus® and HPMCAS-HF was in ratio of (60:20) as optimized by design of experiments study. Moreover, the optimized ASDs batch were stable at 40°C, 75% RH for a period of 6months without any dissolution rate changes, and remained into amorphous state. PMID:27049050

  1. Monodispersed Hollow SO3H-Functionalized Carbon/Silica as Efficient Solid Acid Catalyst for Esterification of Oleic Acid.

    PubMed

    Wang, Yang; Wang, Ding; Tan, Minghui; Jiang, Bo; Zheng, Jingtang; Tsubaki, Noritatsu; Wu, Mingbo

    2015-12-01

    SO3H-functionalized monodispersed hollow carbon/silica spheres (HS/C-SO3H) with primary mesopores were prepared with polystyrene as a template and p-toluenesulfonic acid (TsOH) as a carbon precursor and -SO3H source simultaneously. The physical and chemical properties of HS/C-SO3H were characterized by N2 adsorption, TEM, SEM, XPS, XRD, Raman spectrum, NH3-TPD, element analysis and acid-base titration techniques. As a solid acid catalyst, HS/C-SO3H shows excellent performance in the esterification of oleic acid with methanol, which is a crucial reaction in biodiesel production. The well-defined hollow architecture and enhanced active sites accessibility of HS/C-SO3H guarantee the highest catalytic performance compared with the catalysts prepared by activation of TsOH deposited on the ordered mesoporous silicas SBA-15 and MCM-41. At the optimized conditions, high conversion (96.9%) was achieved and no distinct activity drop was observed after 5 recycles. This synthesis strategy will provide a highly effective solid acid catalyst for green chemical processes. PMID:26588826

  2. Solid-State 17O NMR Study of Benzoic Acid Adsorption On Metal Oxide Surfaces

    SciTech Connect

    Hagaman, Edward {Ed} W; Chen, Banghao; Jiao, Jian; Parsons, Williams

    2012-01-01

    Solid-state 17O NMR spectra of 17O-labeled benzoic and anisic acids are reported and benzoic acid is used to probe the surface of metal oxides. Complexes formed when benzoic acid is dry-mixed with mesoporous silica, and nonporous titania and alumina are characterized. Chemical reactions with silica are not observed. The nature of benzoic acid on silica is a function of the water content of the oxide. The acid disperses in the pores of the silica if the silica is in equilibrium with ambient laboratory humidity. The acid displays high mobility as evidenced by a liquid-like, Lorentzian resonance. Excess benzoic acid remains as the crystalline hydrogen-bonded dimer. Benzoic acid reacts with titania and alumina surfaces in equilibrium with laboratory air to form the corresponding titanium and aluminum benzoates. In both materials the oxygen of the 17O-labeled acid is bound to the metal, showing the reaction proceeds by bond formation between oxygen deficient metal sites and the oxygen of the carboxylic acid. 27Al MAS NMR confirms this mechanism for the reaction on alumina. Dry mixing of benzoic acid with alumina rapidly quenches pentacoordinate aluminum sites, excellent evidence that these sites are confined to the surface of the alumina particles.

  3. Alkene Isomerization Using a Solid Acid as Activator and Support for a Homogeneous Catalyst

    ERIC Educational Resources Information Center

    Seen, Andrew J.

    2004-01-01

    An upper-level undergraduate experiment that, in addition to introducing students to catalysis using an air sensitive transition-metal complex, introduces the use of a solid acid as an activator and support for the catalyst is developed. The increased stability acquired in the course of the process affords the opportunity to characterize the…

  4. Matrix solid-phase dispersion for the liquid chromatographic determination of phenolic acids in Melissa officinalis.

    PubMed

    Ziaková, Alica; Brandsteterová, Eva; Blahová, Eva

    2003-01-01

    Matrix solid-phase dispersion (MSPD) was used for sample preparation of plant material (Melissa officinalis, Lemon Balm) prior to liquid chromatography of rosmarinic, caffeic and protocatechuic acids, phenolic compounds present in this herb. Different MSPD sorbents and various elution agents were tested and the optimal extraction conditions determined with the aim to obtain extraction recoveries greater than 90% for all analytes. PMID:12568390

  5. Sorption of tylosin and sulfamethazine on solid humic acid.

    PubMed

    Guo, Xuetao; Tu, Bei; Ge, Jianhua; Yang, Chen; Song, Xiaomei; Dang, Zhi

    2016-05-01

    Tylosin (TYL) and sulfamethazine (SMT) are ionizable and polar antimicrobial compounds, which have seeped into the environment in substantial amounts via fertilizing land with manure or sewage. Sorption of TYL and SMT onto humic acid (HA) may affect their environmental fate. In this study, the sorption of TYL and SMT on HA at different conditions (pH, ionic strength) was investigated. All sorption isotherms fitted well to the Henry and Freundlich models and they were highly nonlinear with values of n between 0.5 and 0.8, which suggested that the HA had high heterogeneity. The sorption of TYL and SMT on HA decreased with increasing pH (2.0-7.5), implying that the primary sorption mechanism could be due to cation exchange interactions between TYL(+)/SMT(+) species and the functional groups of HA. Increasing ionic strength resulted in a considerable reduction in the Kd values of TYL and SMT, hinting that interactions between H bonds and π-π EDA might be an important factor in the sorption of TYL and SMT on HA. Results of Fourier transform infrared (FT-IR) and (13)C-nuclear magnetic resonance (NMR) analysis further demonstrated that carboxyl groups and O-alkyl structures in the HA could interact with TYL and SMT via ionic interactions and H bonds, respectively. Overall, this work gives new insights into the mechanisms of sorption of TYL and SMT on HA and hence aids us in assessing the environmental risk of TYL and SMT under diverse conditions. PMID:27155426

  6. Direct production of biodiesel from high-acid value Jatropha oil with solid acid catalyst derived from lignin

    PubMed Central

    2011-01-01

    Background Solid acid catalyst was prepared from Kraft lignin by chemical activation with phosphoric acid, pyrolysis and sulfuric acid. This catalyst had high acid density as characterized by scanning electron microscope (SEM), energy-dispersive x-ray spectrometry (EDX) and Brunauer, Emmett, and Teller (BET) method analyses. It was further used to catalyze the esterification of oleic acid and one-step conversion of non-pretreated Jatropha oil to biodiesel. The effects of catalyst loading, reaction temperature and oil-to-methanol molar ratio, on the catalytic activity of the esterification were investigated. Results The highest catalytic activity was achieved with a 96.1% esterification rate, and the catalyst can be reused three times with little deactivation under optimized conditions. Biodiesel production from Jatropha oil was studied under such conditions. It was found that 96.3% biodiesel yield from non-pretreated Jatropha oil with high-acid value (12.7 mg KOH/g) could be achieved. Conclusions The catalyst can be easily separated for reuse. This single-step process could be a potential route for biodiesel production from high-acid value oil by simplifying the procedure and reducing costs. PMID:22145867

  7. Solid solubility in 1:13 phase of doping element for La(Fe,Si)13 alloys

    NASA Astrophysics Data System (ADS)

    Zong, S. T.; Wang, C. L.; Long, Y.; Fu, B.; Shi, J. M.; Han, J.; Zhao, Y. Y.

    2016-05-01

    The influences of Ni, Cr and Nb as substitution elements for Fe were investigated. The change in microstructure and the magnetic properties have been discussed in detail. Substitution elements Ni, Cr and Nb not only have limited solubility in NaZn13-type (1:13) phase, but also hinder the peritectoid reaction. Ni element mainly enters into La-rich phase while Cr element mainly concentrates in α-Fe phase, which both have detriment effect on the peritectoid reaction, leading to a large residual of impurity phases after annealing and a decrease of magnetic entropy change. Besides, Ni and Cr participated in peritectoid reaction by entering parent phases but slightly entering 1:13 phase, which would cause the disappearance of first order magnetic phase transition. A new phase (Fe,Si)2Nb was found when Nb element substitutes Fe in La(Fe,Si)13, suggesting that Nb does not participate in peritectoid reaction and only exists in (Fe,Si)2Nb phase after annealing. The alloy with Nb substitution maintains the first order magnetic phase transition character.

  8. Preparation of solid acid catalyst from glucose-starch mixture for biodiesel production.

    PubMed

    Chen, Guo; Fang, Baishan

    2011-02-01

    The aim of this work is to study the catalyst prepared by glucose-starch mixture. Assessment experiments showed that solid acid behaved the highest esterification activity when glucose and corn powder were mixed at ratio of 1:1, carbonized at 400°C for 75 min and sulfonated with concentrated H(2)SO(4) (98%) at 150°C for 5 h. The catalyst was characterized by acid activity measurement, XPS, TEM and FT-IR. The results indicated that solid acid composed of CS(0.073)O(0.541) has both Lewis acid sites and Bronsted acid sites caused by SO(3)H and COOH. The conversions of oleic acid esterification and triolein transesterification are 96% and 60%, respectively. Catalyst for biodiesel production from waste cottonseed oil containing high free fatty acid (FFA 55.2 wt.%) afforded the methyl ester yield of about 90% after 12h. The catalyst deactivated gradually after recycles usage, but it could be regenerated by H(2)SO(4) treatment. PMID:21067915

  9. A closed loop for municipal organic solid waste by lactic acid fermentation.

    PubMed

    Probst, Maraike; Walde, Janette; Pümpel, Thomas; Wagner, Andreas Otto; Insam, Heribert

    2015-01-01

    In order to investigate the feasibility of producing lactic acid from municipal organic solid waste different pH values (4-7) and temperatures (37°C and 55°C) were tested. For the evaluation of fermentation conditions the chemical, physical, and microbial characters were monitored over a period of 7days. Quantitative real time PCR, PCR-DGGE, and next generation sequencing of a 16S rRNA gene library were applied to identify the key players of the lactic acid production and their association. Lactobacillus acidophilus and its closest relatives were found to be efficient lactic acid producers (>300mM) under most suitable fermentation conditions tested in this study: 37°C with either uncontrolled pH or at a pH of 5. These data provide the first step in the realization of the idea "reuse, reduce, and recycle" of municipal organic solid waste. PMID:25459815

  10. Solid supported in situ derivatization extraction of acidic degradation products of nerve agents from aqueous samples.

    PubMed

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

    2014-09-12

    This study deals with the solid supported in situ derivatization extraction of acidic degradation products of nerve agents present in aqueous samples. Target analytes were alkyl alkylphosphonic acids and alkylphosphonic acids, which are important environmental signatures of nerve agents. The method involved tert-butyldimethylchlorosilane mediated in situ silylation of analytes on commercially available diatomaceous solid phase extraction cartridges. Various parameters such as derivatizing reagent, its concentration, reaction time, temperature and eluting solvent were optimized. Recoveries of the analytes were determined by GC-MS which ranged from 60% to 86%. The limits of detection (LOD) and limit of quantification (LOQ) with selected analytes were achieved down to 78 and 213ngmL(-1) respectively, in selected ion monitoring mode. The successful applicability of method was also demonstrated on samples of biological origin such as plasma and to the samples received in 34th official proficiency test conducted by the Organization for Prohibition the of Chemical Weapons. PMID:25103280

  11. Carbohydrate-Binding Module–Cyclodextrin Glycosyltransferase Fusion Enables Efficient Synthesis of 2-O-d-Glucopyranosyl-l-Ascorbic Acid with Soluble Starch as the Glycosyl Donor

    PubMed Central

    Han, Ruizhi; Li, Jianghua; Shin, Hyun-Dong; Chen, Rachel R.; Du, Guocheng

    2013-01-01

    In this study, we achieved the efficient synthesis of 2-O-d-glucopyranosyl-l-ascorbic acid (AA-2G) from soluble starch by fusing a carbohydrate-binding module (CBM) from Alkalimonas amylolytica α-amylase (CBMAmy) to cyclodextrin glycosyltransferase (CGTase) from Paenibacillus macerans. One fusion enzyme, CGT-CBMAmy, was constructed by fusing the CBMAmy to the C-terminal region of CGTase, and the other fusion enzyme, CGTΔE-CBMAmy, was obtained by replacing the E domain of CGTase with CBMAmy. The two fusion enzymes were then used to synthesize AA-2G from soluble starch as a cheap and easily soluble glycosyl donor. Under the optimal conditions, the AA-2G yields produced using CGTΔE-CBMAmy and CGT-CBMAmy were 2.01 g/liter and 3.03 g/liter, respectively, which were 3.94- and 5.94-fold of the yield from the wild-type CGTase (0.51 g/liter). The reaction kinetics of the two fusion enzymes were analyzed and modeled to confirm the enhanced specificity toward soluble starch. It was also found that, compared to the wild-type CGTase, the two fusion enzymes had relatively high hydrolysis and disproportionation activities, factors that favor AA-2G synthesis. Finally, it was speculated that the enhancement of soluble starch specificity may be related to the changes of substrate binding ability and the substrate binding sites between the CBM and the starch granule. PMID:23503312

  12. Solubility of Organic Compounds

    ERIC Educational Resources Information Center

    James, K. C.

    1972-01-01

    Outlines factors to be considered in choosing suitable solvents for non-electrolytes and salts of weak acids and bases. Describes how, in some simple situation, the degree of solubility can be estimated. (Author/DF)

  13. Solid acid-catalyzed depolymerization of barley straw driven by ball milling.

    PubMed

    Schneider, Laura; Haverinen, Jasmiina; Jaakkola, Mari; Lassi, Ulla

    2016-04-01

    This study describes a time and energy saving, solvent-free procedure for the conversion of lignocellulosic barley straw into reducing sugars by mechanocatalytical pretreatment. The catalytic conversion efficiency of several solid acids was tested which revealed oxalic acid dihydrate as a potential catalyst with high conversion rate. Samples were mechanically treated by ball milling and subsequently hydrolyzed at different temperatures. The parameters of the mechanical treatment were optimized in order to obtain sufficient amount of total reducing sugar (TRS) which was determined following the DNS assay. Additionally, capillary electrophoresis (CE) and Fourier transform infrared spectrometry (FT-IR) were carried out. Under optimal conditions TRS 42% was released using oxalic acid dihydrate as a catalyst. This study revealed that the acid strength plays an important role in the depolymerization of barley straw and in addition, showed, that the oxalic acid-catalyzed reaction generates low level of the degradation product 5-hydroxymethylfurfural (HMF). PMID:26859328

  14. A solid acid esterification catalyst which reduces waste and increases yields

    SciTech Connect

    Lundquist, E.G.

    1993-12-31

    Recent research on polymeric catalysts has led to the development of a new solid acid esterification catalyst which is highly active for the esterification of fatty acids and maleic anhydride at elevated temperatures. The use of this catalyst eliminates the need for a final neutralization step which is required when using traditional homogenous acid (H{sub 2}SO{sub 4} and HCl) catalysts. This neutralization step generates large amounts of waste salts and hurts efficiency since unconsumed organic acid reactants are also neutralized. In the high temperature esterification reactions studied here, the production of dialkyl ether by-products from the acid catalyzed self-condensation of alcohol is also greatly reduced allowing for both high activity and selectivity.

  15. Proton transfer reactions between nitric acid and acetone, hydroxyacetone, acetaldehyde and benzaldehyde in the solid phase.

    PubMed

    Lasne, Jérôme; Laffon, Carine; Parent, Philippe

    2012-12-01

    The heterogeneous and homogeneous reactions of acetone, hydroxyacetone, acetaldehyde and benzaldehyde with solid nitric acid (HNO(3)) films have been studied with Reflection-Absorption Infrared Spectroscopy (RAIRS) under Ultra-High Vacuum (UHV) conditions in the 90-170 K temperature range. In the bulk or at the surface of the films, nitric acid transfers its proton to the carbonyl function of the organic molecules, producing protonated acetone-H(+), hydroxyacetone-H(+), acetaldehyde-H(+) and benzaldehyde-H(+), and nitrate anions NO(3)(-), a reaction not observed when nitric acid is previously hydrated [J. Lasne, C. Laffon and Ph. Parent, Phys. Chem. Chem. Phys., 2012, 14, 697]. This provides a molecular-scale description of the carbonyl protonation reaction in an acid medium, the first step of the acid-catalyzed condensation of carbonyl compounds, fuelling the growth of secondary organic aerosols (SOA) in the atmosphere. PMID:23090634

  16. p-Nitromandelic acid as a highly acid-stable safety-catch linker for solid-phase synthesis of peptide and depsipeptide acids.

    PubMed

    Isidro-Llobet, Albert; Alvarez, Mercedes; Burger, Klaus; Spengler, Jan; Albericio, Fernando

    2007-04-12

    [reaction: see text] p-Nitromandelic acid as a safety-catch linker for Boc/Bzl-SPPS of base-labile compounds like peptides and depsipeptides is described. This linker permits acidic removal of side-chain protection groups from the resin. For cleavage from the solid support, the p-nitro group was reduced with tin(II) chloride. After washing off the reducing agents, the (depsi)peptide acids with or without the side-chain protection schemes were obtained by microwave irradiation at 50 degrees C with 5% TFA in dioxane. PMID:17367151

  17. Synthesis, Chemical and Enzymatic Hydrolysis, and Aqueous Solubility of Amino Acid Ester Prodrugs of 3-Carboranyl Thymidine Analogues for Boron Neutron Capture Therapy of Brain Tumors

    PubMed Central

    Hasabelnaby, Sherifa; Goudah, Ayman; Agarwal, Hitesh K.; Abd alla, Mosaad S. M.; Tjarks, Werner

    2012-01-01

    Various water-soluble L-valine-, L-glutamate-, and glycine ester prodrugs of two 3-Carboranyl Thymidine Analogues (3-CTAs), designated N5 and N5-2OH, were synthesized for Boron Neutron Capture Therapy (BNCT) of brain tumors since the water solubilities of the parental compounds proved to be insufficient in preclinical studies. The amino acid ester prodrugs were prepared and stored as hydrochloride salts. The water solubilities of these amino acid ester prodrugs, evaluated in phosphate buffered saline (PBS) at pH 5, pH 6 and pH 7.4, improved 48 to 6600 times compared with parental N5 and N5-2OH. The stability of the amino acid ester prodrugs was evaluated in PBS at pH 7.4, Bovine serum, and Bovine cerebrospinal fluid (CSF). The rate of the hydrolysis in all three incubation media depended primarily on the amino acid promoiety and, to a lesser extend, on the site of esterification at the deoxyribose portion of the 3-CTAs. In general, 3'-amino acid ester prodrugs were less sensitive to chemical and enzymatic hydrolysis than 5'-amino acid ester prodrugs and the stabilities of the latter decreased in the following order: 5'-valine > 5'-glutamate > 5'-glycine. The rate of the hydrolysis of the 5'-amino acid ester prodrugs in Bovine CSF was overall higher than in PBS and somewhat lower than in Bovine serum. Overall, 5'-glutamate ester prodrug of N5 and the 5'-glycine ester prodrugs of N5 and N5-2OH appeared to be the most promising candidates for preclinical BNCT studies. PMID:22889558

  18. The properties of solid Zn(II)-amino acid complexes in the form of suspensions.

    PubMed

    Dolińska, B

    2001-10-01

    An investigation was made into the experimental conditions for the formation of poorly soluble complexes of the divalent Zinc(II) combined with the following selected amino acids: tyrosine, tryptophan, cysteine, histidine, and alanine, in the form of suspensions for parenteral administration. The number of Zn(II)-binding sites in the amino acid (n) as well as the amino acid affinity to Zn(II) (Ka), were determined. Cysteine was found to have the highest number of Zn(II)-binding sites--3, whereas alanine the lowest--1. In the conditions described herein, Zn(II) amino acid complexes of diverse stability (durability) were obtained. The analysis of the kinetics of the binding revealed that the most stable complexes were those formed by Zn(II) in combination with tryptophan (Ka = 405.78 microM(-1) +/- 12.17), and with tyrosine (Ka = 343.88 microM +/- 22.35); whereas the least stable complexes were those formed by Zn(II) in combination with histidine (Ka = 29.90 microM +/- 4.78), and with alanine (Ka = 13.0 microM(-1) +/- 1.04). Cysteine formed complexes of intermediate stability (Ka = 168.53 microM(-1) +/- 12.36). The stability ofthe Zn(II) amino acid complexes obtained was conditioned by both the molecular weight (P = 0.033) of the amino acid and its isoelectric point (P < 0.001). PMID:11718265

  19. Characterization and Soluble Expression of D-Hydantoinase from Pseudomonas fluorescens for the Synthesis of D-Amino Acids.

    PubMed

    Xu, Guo-Chao; Li, Lei; Han, Rui-Zhi; Dong, Jin-Jun; Ni, Ye

    2016-04-01

    An active D-hydantoinase from Pseudomonas fluorescens was heterogeneously overexpressed in Escherichia coli BL21(DE3) and designated as D-PfHYD. Sequence and consensus analysis suggests that D-PfHYD belongs to the dihydropyrimidinase/hydantoinase family and possesses catalytic residues for metal ion and hydantoin binding. D-PfHYD was purified to homogeneity by nickel affinity chromatography for characterization. D-PfHYD is a homotetramer with molecular weight of 215 kDa and specific activity of 20.9 U mg(-1). D-PfHYD showed the highest activity at pH 9.0 and 60 °C. Metal ions such as Mn(2+), Fe(2+), and Fe(3+) could activate D-PfHYD with 20 % improvement. Substrate specificity analysis revealed that purified D-PfHYD preferred aliphatic to aromatic 5'-monosubstituted hydantoins. Among various strategies tested, chaperone GroES-GroEL was efficient in improving the soluble expression of D-PfHYD. Employing 1.0 g L(-1) recombinant E. coli BL21(DE3)-pET28-hyd/pGRO7 dry cells, 100 mM isobutyl hydantoin was converted into D-isoleucine with 98.7 % enantiomeric excess (ee), isolation yield of 78.3 %, and substrate to biocatalyst ratio of 15.6. Our results suggest that recombinant D-PfHYD could be potentially applied in the synthesis of D-amino acids. PMID:26821258

  20. Short communication: Effect of conjugated linoleic acid on concentrations of fat-soluble vitamins in milk of lactating ewes.

    PubMed

    Zeitz, J O; Most, E; Eder, K

    2015-10-01

    Conjugated linoleic acids (CLA) are well known as milk fat-reducing feed supplements in diets for lactating ruminants. However, their effects on milk concentrations of fat-soluble vitamins are unknown. This study was performed to investigate the hypothesis that CLA affect the concentrations of retinol and tocopherol in ewe milk. For that purpose, group-housed Merino ewes (101 ± 13.7 kg) nursing twin lambs and fed with a hay:concentrate diet were supplemented with either 45 g of a rumen-protected CLA supplement containing 3.4 g of cis-9,trans-11-CLA and 3.4 g of trans-10,cis-12-CLA (CLA group, n=11) or with 45 g of a hydrogenated vegetable fat (control group, n=12) per ewe per day during the first 6 wk of lactation. Feed intake was recorded daily (concentrate) or weekly (hay) per group. Milk spot samples were collected at the beginning of the experiment (5 ± 2.4 d postpartum) and then weekly after lambs had been separated for 2 h from their mothers. The milk fat content was determined and feed and milk were analyzed for concentrations of α-, γ-, and δ-tocopherol and for retinol by HPLC. Dietary intake of tocopherol and retinol was similar in both groups. Feeding CLA decreased milk fat concentration by 23% on average, and during the first 3 wk of the study milk tocopherol concentration tended to be increased by feeding CLA (+17%), but retinol concentrations were not influenced. When related to milk fat, CLA feeding significantly increased both milk tocopherol (+40%) and retinol (+32%) and these effects were evident during the whole experimental period corresponding to the first half of lactation. PMID:26254518

  1. Hydrothermal preparation and characterization of novel corncob-derived solid acid catalysts.

    PubMed

    Ma, Huan; Li, Jiabao; Liu, Weiwei; Cheng, Beijiu; Cao, Xiaoyan; Mao, Jingdong; Zhu, Suwen

    2014-06-11

    Novel corncob-derived solid acid catalysts were successfully synthesized for the first time by the hydrothermal method. The influences of different preparation conditions were investigated, and the structure-function relationships of the resulting catalysts were also discussed on the basis of the analysis of structure and composition. In comparison to conventional solid acid catalysts, the corncob-derived catalyst synthesized under optimized conditions exhibited higher catalytic activity in esterification reactions, yielding nearly 90% methyl oleate in only 2 h. The catalyst retained satisfactory catalytic activity for esterification, even after 8 reaction cycles. Solid-state magic angle spinning (MAS) (13)C nuclear magnetic resonance (NMR) investigations further indicated that the catalyst was composed of polycyclic aromatic carbon sheets bearing -SO3H, -COOH, and -OH groups in adequate amounts and with proper proportions, contributing to its excellent catalytic activity. This work provides a green method to synthesize solid acid catalysts from biomass wastes and may contribute to a holistic approach for biomass conversion. PMID:24820344

  2. Microstructure, excess solid solubility, and elevated-temperature mechanical behavior of spray-atomized and codeposited Al-Ti-SiCP

    NASA Astrophysics Data System (ADS)

    Gupta, M.; Juarez-Islas, J.; Frazier, W. E.; Mohamed, F. A.; Lavernia, E. J.

    1992-12-01

    In the present study, the microstructure, thermal stability, and elevated temperature mechanical behavior of Al-Ti-SiCP metal matrix composites (MMCs) processed by spray atomization and codeposition were investigated. The evolution of the microstructure of the spray-deposited material before and after thermal annealing was studied using X-ray diffractometry, transmission electron microscopy (TEM), scanning electron microscopy (SEM), and optical microscopy. The thermal stability of the spray-deposited materials was determined by monitoring the changes in hardness after isochronal thermal anneals at various temperatures. The results of X-ray and microanalysis studies revealed the presence of a supersaturated solid solution of Ti in α Al in the spray-atomized and codeposited material, with Ti concentrations in the 0.8 to 1.1 wt pet range. The formation of an extended solid solution was discussed in light of the cooling rates present during atomization and, subsequently, during deposition. Regarding mechanical behavior, the present results suggest that the as-spray deposited and hot extruded Al-Ti matrix is thermally stable up to a temperature of 400 °C and that the excess solid solubility of Ti in a Al, resulting from the rapid quench during processing, is maintained up to a temperature of 300 °C. The elevated-temperature mechanical properties of the hot extruded spray-deposited materials were studied following a 100-hour exposure at 250 °C, 350 °C, and 450 °C; the roomtemperature mechanical properties were also determined. Results show that the elevated-temperature yield strength of the spray-deposited and extruded materials compared favorably to those of an equivalent alloy made by powder metallurgical materials, were superior to those of the ingot material, but were inferior to those of mechanically alloyed Al-Ti materials. In addition, TEM studies showed no evidence of interfacial reactions at the Al-Ti/SiCP interface.

  3. Radionuclide Leaching from Residual Solids Remaining after Acid Dissolution of Composite K East Canister Sludge

    SciTech Connect

    Delegard, C.H.; Rinehart, D.E.; Soderquist, C.Z.; Fadeff, S.K.

    1999-04-02

    Laboratory tests were performed to examine mixed nitric/hydrofluoric acid leach treatments for decontaminating dissolver residual solids (KECDVSR24H-2) produced during a 20- to 24-hr dissolution of a composite K East (KE) Basin canister sludge in 95 C 6 M nitric acid (HNO{sub 3}). The scope of this testing has been described in Section 4.5 of ''Testing Strategy to Support the Development of K Basin Sludge Treatment Process'' (Flament 1998). Radionuclides sorbed or associated with the residual solids generated in the K Basin sludge treatment process can restrict disposal of this solid to the Environmental Restoration Disposal Facility (ERDF). The starting dissolver residual solid for this testing, KECDVSR24H-2, contains radionuclides at concentrations which exceed the ERDF Waste Acceptance Criteria for TRU by about a factor of 70, for {sup 239}Pu by a factor of 200, and for {sup 241}Am by a factor of 50. The solids also exceed the ERDF criterion for {sup 137}Cs by a factor of 2 and uranium by a factor of 5. Therefore, the radionuclides of greatest interest in this leaching study are first {sup 239}Pu and {sup 241}Am (both components of TRU) and then uranium and {sup 137}Cs.

  4. Particulate organic acids and overall water-soluble aerosol composition measurements from the 2006 Gulf of Mexico Atmospheric Composition and Climate Study (GoMACCS)

    NASA Astrophysics Data System (ADS)

    Sorooshian, Armin; Ng, Nga L.; Chan, Arthur W. H.; Feingold, Graham; Flagan, Richard C.; Seinfeld, John H.

    2007-07-01

    The Center for Interdisciplinary Remotely-Piloted Aircraft Studies (CIRPAS) Twin Otter participated in the Gulf of Mexico Atmospheric Composition and Climate Study (GoMACCS) mission during August-September 2006. A particle-into-liquid sampler (PILS) coupled to ion chromatography was used to characterize the water-soluble ion composition of aerosol and cloud droplet residual particles (976 5-min PM1.0 samples in total). Sulfate and ammonium dominated the water-soluble mass (NH4+ + SO42- = 84 ± 14%), while organic acids contributed 3.4 ± 3.7%. The average NH4+:SO42- molar ratio was 1.77 ± 0.85. Particulate concentrations of organic acids increased with decreasing carbon number from C9 to C2. Organic acids were most abundant above cloud, presumably as a result of aqueous phase chemistry in cloud droplets, followed by subsequent droplet evaporation above cloud tops; the main product of this chemistry was oxalic acid. The evolution of organic acids with increasing altitude in cloud provides evidence for the multistep nature of oxalic acid production; predictions from a cloud parcel model are consistent with the observed oxalate:glyoxylate ratio as a function of altitude in GoMACCS cumuli. Suppressed organic acid formation was observed in clouds with relatively acidic droplets, as determined by high particulate nitrate concentrations (presumably high HNO3 levels too) and lower liquid water content, as compared to other cloud fields probed. In the Houston Ship Channel region, an area with significant volatile organic compound emissions, oxalate, acetate, formate, benzoate, and pyruvate, in decreasing order, were the most abundant organic acids. Photo-oxidation of m-xylene in laboratory chamber experiments leads to a particulate organic acid product distribution consistent with the Ship Channel area observations.

  5. Conversion of carbohydrate biomass to γ-valerolactone by using water-soluble and reusable iridium complexes in acidic aqueous media.

    PubMed

    Deng, Jin; Wang, Yan; Pan, Tao; Xu, Qing; Guo, Qing-Xiang; Fu, Yao

    2013-07-01

    Mild-mannered manipulation: A catalytic method for the conversion of carbohydrate biomass to γ-valerolactone in acidic aqueous media has been developed. The water-soluble iridium complexes were observed to be extremely catalytically active for providing γ-valerolactone in high yields with high TONs. The homogeneous catalysts can also be recycled and reused by applying a simple phase separation process. PMID:23757330

  6. Short communication: Effects of molasses products on productivity and milk fatty acid profile of cows fed diets high in dried distillers grains with solubles.

    PubMed

    Siverson, A; Vargas-Rodriguez, C F; Bradford, B J

    2014-01-01

    Previous research has shown that replacing up to 5% [of dietary dry matter (DM)] corn with cane molasses can partially alleviate milk fat depression when cows are fed high-concentrate, low-fiber rations containing dried distillers grains with solubles. The primary objective of this study was to determine whether dietary molasses alters milk fatty acid (FA) profile or improves solids-corrected milk yield in the context of a more typical lactation diet. A secondary objective was to assess production responses to increasing rumen-degradable protein supply when molasses was fed. Twelve primiparous and 28 multiparous Holstein cows (196 ± 39 d in milk) were blocked by parity and assigned to 4 pens. Pens were randomly allocated to treatment sequence in a 4 × 4 Latin square design, balanced for carryover effects. Treatment periods were 21 d, with 17 d for diet adaptation and 4 d for sample and data collection. Treatments were a control diet, providing 20% dried distillers grains with solubles (DM basis), 35% neutral detergent fiber, 30% starch, and 5% ether extract; a diet with 4.4% cane molasses replacing a portion of the corn grain; a diet with 2.9% molasses supplement containing 32% crude protein on a DM basis; and a diet with 5.8% (DM basis) molasses supplement. Animal-level data were analyzed using mixed models, including the fixed effect of treatment and the random effects of period, pen, period × pen interaction, and cow within pen to recognize pen as the experimental unit. Diets did not alter DM intake, milk production, milk component concentration or yield, feed efficiency (DM intake/milk yield), body weight change, or milk somatic cell count. Milk stearic acid content was increased by the diet containing 5.8% molasses supplement compared with the control diet and the diet containing 2.9% molasses supplement, but the magnitude of the effect was small (12.27, 11.75, and 11.69 ± 0.29 g/100g of FA). Production data revealed a dramatic effect of period on milk fat

  7. Solid-Phase Spectrophotometric Analysis of 1-Naphthol Using Silica Functionalized with m-Diazophenylarsonic Acid.

    PubMed

    Zaitseva, Nataliya; Alekseev, Sergei; Zaitsev, Vladimir; Raks, Viktoria

    2016-12-01

    The m-aminophenylarsonic acid (m-APAA) was immobilized onto the silica gel surface with covalently grafted quaternary ammonium groups via ion exchange. The diazotization of ion-bonded m-APAA resulted in a new solid-phase spectrophotometric reagent for detection of 1-naphtol in environmental water samples. The procedure of solid-phase spectrophotometric analysis is characterized by 20 μg L(-1) limit of detection (LOD) of 1-naphtol, up to 2000 concentration factor, and insensitivity to the presence of natural water components as well as to 30-fold excess of phenol, resorcinol, and catechol. PMID:26979727

  8. Solid-Phase Spectrophotometric Analysis of 1-Naphthol Using Silica Functionalized with m-Diazophenylarsonic Acid

    NASA Astrophysics Data System (ADS)

    Zaitseva, Nataliya; Alekseev, Sergei; Zaitsev, Vladimir; Raks, Viktoria

    2016-03-01

    The m-aminophenylarsonic acid (m-APAA) was immobilized onto the silica gel surface with covalently grafted quaternary ammonium groups via ion exchange. The diazotization of ion-bonded m-APAA resulted in a new solid-phase spectrophotometric reagent for detection of 1-naphtol in environmental water samples. The procedure of solid-phase spectrophotometric analysis is characterized by 20 μg L-1 limit of detection (LOD) of 1-naphtol, up to 2000 concentration factor, and insensitivity to the presence of natural water components as well as to 30-fold excess of phenol, resorcinol, and catechol.

  9. Preparation of solid drug/cyclodextrin complexes of acidic and basic drugs.

    PubMed

    Loftsson, T; Sigurdsson, H H; Másson, M; Schipper, N

    2004-01-01

    One of the main obstacles in pharmaceutical applications of cyclodextrins is their increase of the formulation bulk. Even at maximum incorporation 500 mg of a solid drug/cyclodextrin complex will only contain between 50 and 125 mg of the drug, assuming a low molecular weight drug (MW 200 to 400 Dalton) and an average molecular weight cyclodextrin (MW about 1500 Dalton). In general, the complexation efficiency is low and consequently the complex powder contains a significant amount of empty cyclodextrin molecules. In the present study the complexation efficiency is increased by ionization of the drug molecule through addition of volatile acid (i.e. acetic acid) or base (i.e. ammonia) to the aqueous complexation media of basic or acidic drugs, respectively. The volatile acid or base was then removed during lyophilization and heating in a vacuum oven resulting in formation of solid cyclodextrin complexes of the unionized drug. Thus, the complexation efficiency was temporary increased by the ionization but then again decreased leading to formation of the thermodynamically unstable solid drug/cyclodextrin complexes. When dissolved the energy of the system was lowered by expelling the drug molecules from the cyclodextrin cavities resulting in formation of supersaturated drug solutions and ultimately precipitation of the drug. PMID:14964417

  10. Development of micro-fibrous solid dispersions of poorly water-soluble drugs in sucrose using temperature-controlled centrifugal spinning

    PubMed Central

    Marano, Stefania; Barker, Susan Anne; Raimi-Abraham, Bahijja Tolulope; Missaghi, Shahrzad; Rajabi-Siahboomi, Ali; Craig, Duncan Q.M.

    2016-01-01

    Solid dispersion technology represents a successful approach to addressing the bioavailability issues caused by the low aqueous solubility of many Biopharmaceutics Classification System (BCS) Class II drugs. In this study, the use of high-yield manufacture of fiber-based dispersion is explored as an alternative approach to monolith production methods. A temperature-controlled solvent-free centrifugal spinning process was used to produce sucrose-based microfibers containing the poorly water-soluble drugs olanzapine and piroxicam (both BCS Class II); these were successfully incorporated into the microfibers and the basic characteristics of fiber diameter, glassy behavior, drug loading capacity and drug–sucrose interaction assessment were measured. Scanning electron microscopy revealed that bead-free drug-loaded microfibers with homogenous morphology and diameter in the range of a few micrometers were prepared using our process. Differential scanning calorimetric and X-ray diffraction analyses showed that both drug and carrier were present in the amorphous state in the microfibers, although in the case of piroxicam-loaded microfibers, the presence of small amounts of crystalline drug was observed under polarized light microscopy and in Fourier transform infrared spectra. Drug dissolution performance was evaluated under both sink and non-sink conditions and was found to be significantly enhanced compared to the corresponding crystalline physical mixtures and pure drugs, with evidence of supersaturation behavior noted under non-sink conditions. This study has demonstrated that microfiber-based dispersions may be manufactured by the centrifugal spinning process and may possess characteristics that are favorable for the enhanced dissolution and oral absorption of drugs. PMID:27012901

  11. Development of micro-fibrous solid dispersions of poorly water-soluble drugs in sucrose using temperature-controlled centrifugal spinning.

    PubMed

    Marano, Stefania; Barker, Susan Anne; Raimi-Abraham, Bahijja Tolulope; Missaghi, Shahrzad; Rajabi-Siahboomi, Ali; Craig, Duncan Q M

    2016-06-01

    Solid dispersion technology represents a successful approach to addressing the bioavailability issues caused by the low aqueous solubility of many Biopharmaceutics Classification System (BCS) Class II drugs. In this study, the use of high-yield manufacture of fiber-based dispersion is explored as an alternative approach to monolith production methods. A temperature-controlled solvent-free centrifugal spinning process was used to produce sucrose-based microfibers containing the poorly water-soluble drugs olanzapine and piroxicam (both BCS Class II); these were successfully incorporated into the microfibers and the basic characteristics of fiber diameter, glassy behavior, drug loading capacity and drug-sucrose interaction assessment were measured. Scanning electron microscopy revealed that bead-free drug-loaded microfibers with homogenous morphology and diameter in the range of a few micrometers were prepared using our process. Differential scanning calorimetric and X-ray diffraction analyses showed that both drug and carrier were present in the amorphous state in the microfibers, although in the case of piroxicam-loaded microfibers, the presence of small amounts of crystalline drug was observed under polarized light microscopy and in Fourier transform infrared spectra. Drug dissolution performance was evaluated under both sink and non-sink conditions and was found to be significantly enhanced compared to the corresponding crystalline physical mixtures and pure drugs, with evidence of supersaturation behavior noted under non-sink conditions. This study has demonstrated that microfiber-based dispersions may be manufactured by the centrifugal spinning process and may possess characteristics that are favorable for the enhanced dissolution and oral absorption of drugs. PMID:27012901

  12. Anti-glioma activity and the mechanism of cellular uptake of asiatic acid-loaded solid lipid nanoparticles.

    PubMed

    Garanti, Tanem; Stasik, Aneta; Burrow, Andrea Julie; Alhnan, Mohamed A; Wan, Ka-Wai

    2016-03-16

    Asiatic acid (AA), a pentacyclic triterpene found in Centella Asiatica, has shown neuroprotective and anti-cancer activity against glioma. However, owing to its poor aqueous solubility, effective delivery and absorption across biological barriers, in particular the blood brain barrier (BBB), are challenging. Solid lipid nanoparticles (SLNs) have shown a promising potential as a drug delivery system to carry lipophilic drugs across the BBB, a major obstacle in brain cancer therapy. Nevertheless, limited information is available about the cytotoxic mechanisms of nano-lipidic carriers with AA on normal and glioma cells. This study assessed the anti-cancer efficacy of AA-loaded SLNs against glioblastoma and their cellular uptake mechanism in comparison with SVG P12 (human foetal glial) cells. SLNs were systematically investigated for three different solid lipids; glyceryl monostearate (MS), glyceryl distearate (DS) and glyceryl tristearate (TS). The non-drug containing MS-SLNs (E-MS-SLNs) did not show any apparent toxicity towards normal SVG P12 cells, whilst the AA-loaded MS-SLNs (AA-MS-SLNs) displayed a more favourable drug release profile and higher cytotoxicity towards U87 MG cells. Therefore, MS-SLNs were chosen for further in vitro studies. Cytotoxicity studies of SLNs (± AA) were performed using MTT assay where AA-SLNs showed significantly higher cytotoxicity towards U87 MG cells than SVG P12 normal cells, as confirmed by flow cell cytometry. Cellular uptake of SLNs also appeared to be preferentially facilitated by energy-dependent endocytosis as evidenced by fluorescence imaging and flow cell cytometry. Using the Annexin V-PI double staining technique, it was found that these AA-MS-SLNs displayed concentration-dependent apoptotic activity on glioma cells, which further confirms the potential of exploiting these AA-loaded MS-SLNs for brain cancer therapy. PMID:26775062

  13. Zoledronic acid increases the circulating soluble RANKL level in mice, with a further increase in lymphocyte-derived soluble RANKL in zoledronic acid- and glucocorticoid-treated mice stimulated with bacterial lipopolysaccharide.

    PubMed

    Abe, Takahiro; Sato, Tsuyoshi; Kokabu, Shoichiro; Hori, Naoko; Shimamura, Yumiko; Sato, Tomoya; Yoda, Tetsuya

    2016-07-01

    The nitrogen-containing bisphosphonate (BP) zoledronic acid (ZA) is a potent antiresorptive drug used in conjunction with standard cancer therapy to treat osteolysis or hypercalcemia due to malignancy. However, it is unclear how ZA influences the circulating levels of bone remodeling factors. The aim of this study was to evaluate the effects of ZA on the serum levels of soluble receptor activator of NF-kB ligand (sRANKL) and osteoprotegerin (OPG). The following four groups of C57BL/6 mice were used (five mice per group): (1) the placebo+phosphate-buffered saline (PBS) group, in which placebo-treated mice were injected once weekly with PBS for 4weeks; (2) the placebo+ZA group, in which placebo-treated mice were injected once weekly with ZA for 4weeks; (3) the prednisolone (PSL)+PBS group, in which PSL-treated mice were injected once weekly with PBS for 4weeks; and (4) the PSL+ZA group, in which PSL-treated mice were injected once weekly with ZA for 4weeks. At the 3-week time point, all mice were subjected to oral inflammatory stimulation with bacterial lipopolysaccharide (LPS). The sera of these mice were obtained every week and the levels of sRANKL and OPG were measured using enzyme-linked immunosorbent assay. At the time of sacrifice, femurs were prepared for micro-computed tomography (micro-CT), histological, and histomorphometric analyses. Our data indicated that ZA administration remarkably reduced bone turnover and significantly increased the basal level of sRANKL. Interestingly, the PSL+ZA group showed a dramatically elevated sRANKL level after LPS stimulation. In contrast, the PSL+ZA group in nonobese diabetic mice with severe combined immunodeficiency disease (NOD-SCID mice), which are characterized by the absence of functional T- and B-lymphocytes, showed no increase in the sRANKL level. Our data suggest that, particularly with combination treatment of ZA and glucocorticoids, surviving lymphocytes might be the source of inflammation-induced sRANKL. Thus

  14. Solid Polymer Electrolytes Based on Functionalized Tannic Acids from Natural Resources for All-Solid-State Lithium-Ion Batteries.

    PubMed

    Shim, Jimin; Bae, Ki Yoon; Kim, Hee Joong; Lee, Jin Hong; Kim, Dong-Gyun; Yoon, Woo Young; Lee, Jong-Chan

    2015-12-21

    Solid polymer electrolytes (SPEs) for all-solid-state lithium-ion batteries are prepared by simple one-pot polymerization induced by ultraviolet (UV) light using poly(ethylene glycol) methyl ether methacrylate (PEGMA) as an ion-conducting monomeric unit and tannic acid (TA)-based crosslinking agent and plasticizer. The crosslinking agent and plasticizer based on natural resources are obtained from the reaction of TA with glycidyl methacrylate and glycidyl poly(ethylene glycol), respectively. Dimensionally stable free-standing SPE having a large ionic conductivity of 5.6×10(-4)  Scm(-1) at room temperature can be obtained by the polymerization of PEGMA into P(PEGMA) with a very small amount (0.1 wt %) of the crosslinking agent and 2.0 wt % of the plasticizer. The ionic conductivity value of SPE with a crosslinked structure is one order of magnitude larger than that of linear P(PEGMA) in the waxy state. PMID:26609912

  15. Synthesis of sulfonated porous carbon nanospheres solid acid by a facile chemical activation route

    SciTech Connect

    Chang, Binbin Guo, Yanzhen; Yin, Hang; Zhang, Shouren; Yang, Baocheng

    2015-01-15

    Generally, porous carbon nanospheres materials are usually prepared via a template method, which is a multi-steps and high-cost strategy. Here, we reported a porous carbon nanosphere solid acid with high surface area and superior porosity, as well as uniform nanospheical morphology, which prepared by a facile chemical activation with ZnCl{sub 2} using resorcinol-formaldehyde (RF) resins spheres as precursor. The activation of RF resins spheres by ZnCl{sub 2} at 400 °C brought high surface area and large volume, and simultaneously retained numerous oxygen-containing and hydrogen-containing groups due to the relatively low processing temperature. The presence of these functional groups is favorable for the modification of –SO{sub 3}H groups by a followed sulfonation treating with sulphuric acid and organic sulfonic acid. The results of N{sub 2} adsorption–desorption and electron microscopy clearly showed the preservation of porous structure and nanospherical morphology. Infrared spectra certified the variation of surface functional groups after activation and the successful modification of –SO{sub 3}H groups after sulfonation. The acidities of catalysts were estimated by an indirect titration method and the modified amount of –SO{sub 3}H groups were examined by energy dispersive spectra. The results suggested sulfonated porous carbon nanospheres catalysts possessed high acidities and –SO{sub 3}H densities, which endowed their significantly catalytic activities for biodiesel production. Furthermore, their excellent stability and recycling property were also demonstrated by five consecutive cycles. - Graphical abstract: Sulfonated porous carbon nanospheres with high surface area and superior catalytic performance were prepared by a facile chemical activation route. - Highlights: • Porous carbon spheres solid acid prepared by a facile chemical activation. • It owns high surface area, superior porosity and uniform spherical morphology. • It possesses

  16. Prototype demonstration of dual sorbent injection for acid gas control on municipal solid waste combustion units

    SciTech Connect

    1994-05-01

    This report gathered and evaluated emissions and operations data associated with furnace injection of dry hydrated lime and duct injection of dry sodium bicarbonate at a commercial, 1500 ton per day, waste-to-energy facility. The information compiled during the project sheds light on these sorbents to affect acid gas emissions from municipal solid waste combustors. The information assesses the capability of these systems to meet the 1990 Clean Air Act and 1991 EPA Emission Guidelines.

  17. Solid-State NMR Characterization of Mixed Phosphonic Acid Ligand Binding and Organization on Silica Nanoparticles.

    PubMed

    Davidowski, Stephen K; Holland, Gregory P

    2016-04-01

    As ligand functionalization of nanomaterials becomes more complex, methods to characterize the organization of multiple ligands on surfaces is required. In an effort to further the understanding of ligand-surface interactions, a combination of multinuclear ((1)H, (29)Si, (31)P) and multidimensional solid-state nuclear magnetic resonance (NMR) techniques was utilized to characterize the phosphonic acid functionalization of fumed silica nanoparticles using methylphosphonic acid (MPA) and phenylphosphonic acid (PPA). (1)H → (29)Si cross-polarization (CP)-magic angle spinning (MAS) solid-state NMR was used to selectively detect silicon atoms near hydrogen atoms (primarily surface species); these results indicate that geminal silanols are preferentially depleted during the functionalization with phosphonic acids. (1)H → (31)P CP-MAS solid-state NMR measurements on the functionalized silica nanoparticles show three distinct resonances shifted upfield (lower ppm) and broadened compared to the resonances of the crystalline ligands. Quantitative (31)P MAS solid-state NMR measurements indicate that ligands favor a monodentate binding mode. When fumed silica nanoparticles were functionalized with an equal molar ratio of MPA and PPA, the MPA bound the nanoparticle surface preferentially. Cross-peaks apparent in the 2D (1)H exchange spectroscopy (EXSY) NMR measurements of the multiligand sample at short mixing times indicate that the MPA and PPA are spatially close (≤5 Å) on the surface of the nanostructure. Furthermore, (1)H-(1)H double quantum-single quantum (DQ-SQ) back-to-back (BABA) 2D NMR spectra further confirmed that MPA and PPA are strongly dipolar coupled with observation of DQ intermolecular contacts between the ligands. DQ experimental buildup curves and simulations indicate that the average distance between MPA and PPA is no further than 4.2 ± 0.2 Å. PMID:26914738

  18. Malate Plays a Crucial Role in Starch Metabolism, Ripening, and Soluble Solid Content of Tomato Fruit and Affects Postharvest Softening[W][OA

    PubMed Central

    Centeno, Danilo C.; Osorio, Sonia; Nunes-Nesi, Adriano; Bertolo, Ana L.F.; Carneiro, Raphael T.; Araújo, Wagner L.; Steinhauser, Marie-Caroline; Michalska, Justyna; Rohrmann, Johannes; Geigenberger, Peter; Oliver, Sandra N.; Stitt, Mark; Carrari, Fernando; Rose, Jocelyn K.C.; Fernie, Alisdair R.

    2011-01-01

    Despite the fact that the organic acid content of a fruit is regarded as one of its most commercially important quality traits when assessed by the consumer, relatively little is known concerning the physiological importance of organic acid metabolism for the fruit itself. Here, we evaluate the effect of modifying malate metabolism in a fruit-specific manner, by reduction of the activities of either mitochondrial malate dehydrogenase or fumarase, via targeted antisense approaches in tomato (Solanum lycopersicum). While these genetic perturbations had relatively little effect on the total fruit yield, they had dramatic consequences for fruit metabolism, as well as unanticipated changes in postharvest shelf life and susceptibility to bacterial infection. Detailed characterization suggested that the rate of ripening was essentially unaltered but that lines containing higher malate were characterized by lower levels of transitory starch and a lower soluble sugars content at harvest, whereas those with lower malate contained higher levels of these carbohydrates. Analysis of the activation state of ADP-glucose pyrophosphorylase revealed that it correlated with the accumulation of transitory starch. Taken together with the altered activation state of the plastidial malate dehydrogenase and the modified pigment biosynthesis of the transgenic lines, these results suggest that the phenotypes are due to an altered cellular redox status. The combined data reveal the importance of malate metabolism in tomato fruit metabolism and development and confirm the importance of transitory starch in the determination of agronomic yield in this species. PMID:21239646

  19. Determination of total antioxidant capacity of humic acids using CUPRAC, Folin-Ciocalteu, noble metal nanoparticle- and solid-liquid extraction-based methods.

    PubMed

    Karadirek, Şeyda; Kanmaz, Nergis; Balta, Zeynep; Demirçivi, Pelin; Üzer, Ayşem; Hızal, Jülide; Apak, Reşat

    2016-06-01

    Total antioxidant capacity (TAC) of humic acid (HA) samples was determined using CUPRAC (CUPric Reducing Antioxidant Capacity), FC (Folin-Ciocalteu), QUENCHER-CUPRAC, QUENCHER-FC, Ag-NP (Silver nanoparticle)‒ and Au-NP (Gold nanoparticle)‒based methods. Conventional FC and modified FC (MFC) methods were applied to solid samples. Because of decreased solubility of Folin-Ciocalteu's phenol reagent in organic solvents, solvent effect on TAC measurement was investigated using QUENCHER-CUPRAC assay by using ethanol:distilled water and dimethyl sulfoxide:distilled water with varying ratios. To see the combined effect of solubilization (leaching) and TAC measurement of humic acids simultaneously, QUENCHER experiments were performed at 25°C and 50°C; QUENCHER-CUPRAC and QUENCHER-FC methods agreed well and had similar precision in F-statistics. Although the Gibbs free energy change (ΔG°) of the oxidation of HA dihydroxy phenols with the test reagents were negative, the ΔG° was positive only for the reaction of CUPRAC reagent with isolated monohydric phenols, showing CUPRAC selectivity toward polyphenolic antioxidants. This is the first work on the antioxidant capacity measurement of HA having a sparingly soluble matrix where enhanced solubilization of bound phenolics is achieved with coupled oxidation by TAC reagents. PMID:27130098

  20. Strategies to achieve high-solids enzymatic hydrolysis of dilute-acid pretreated corn stover.

    PubMed

    Geng, Wenhui; Jin, Yongcan; Jameel, Hasan; Park, Sunkyu

    2015-01-01

    Three strategies were presented to achieve high solids loading while maximizing carbohydrate conversion, which are fed-batch, splitting/thickening, and clarifier processes. Enzymatic hydrolysis was performed at water insoluble solids (WIS) of 15% using washed dilute-acid pretreated corn stover. The carbohydrate concentration increased from 31.8 to 99.3g/L when the insoluble solids content increased from 5% to 15% WIS, while the final carbohydrate conversion was decreased from 78.4% to 73.2%. For the fed-batch process, a carbohydrate conversion efficiency of 76.8% was achieved when solid was split into 60:20:20 ratio, with all enzymes added first. For the splitting/thickening process, a carbohydrate conversion of 76.5% was realized when the filtrate was recycled to simulate a steady-state process. Lastly, the clarifier process was evaluated and the highest carbohydrate conversion of 81.4% was achieved. All of these results suggests the possibility of enzymatic hydrolysis at high solids to make the overall conversion cost-competitive. PMID:25836373

  1. A new maleimide-bound acid-cleavable solid-support reagent for profiling phosphorylation.

    PubMed

    Chowdhury, Saiful M; Munske, Gerhard R; Siems, William F; Bruce, James E

    2005-01-01

    A new chemical strategy for phosphopeptide profiling is reported in this study. Phosphorylation represents one of the most important classes of posttranslational modifications of proteins. Here we report a generalized strategy that employs solid-phase capture and mass-encoding steps to selectively enrich phosphopeptides from complex mixtures. This method exploits conversion of phosphates into thiols and reactive compounds to selectively isolate products of phosphorylation. Selective isolation of phosphopeptides is achieved with a simple, novel, acid-cleavable, solid-support-bound maleimide reagent. Our chemistry efforts have focused on minimization of linker size and simplification of reagent production with incorporation of common solid-phase peptide synthesis steps. Relative quantitation was demonstrated by modifying phosphopeptides with incorporation of ethanedithiol and propanedithiol. We observed that appropriate normalization is necessary to utilize mass tag strategies for relative quantitation of posttranslational modifications. The utility of solid-phase capture was determined with model phosphopeptides, and the method was demonstrated with enriching phosphopeptides from beta-casein, alpha-casein and ovalbumin. The solid-phase capture and release methods were also demonstrated with unfractionated whole histone protein mixtures to show this compound applicability in real biological samples. The new chemical strategy will ultimately be utilized for high-throughput profiling of phosphorylation and possibly other posttranslational modifications. PMID:15739244

  2. Water-soluble polymeric chemosensor for selective detection of Hg(2+) in aqueous solution using rhodamine-based modified poly(acrylamide-acrylic acid).

    PubMed

    Geng, Tong-Mou; Wu, Da-Yu

    2015-12-01

    We report the fabrication of a novel easily available turn-on fluorescent water-soluble polymeric chemosensor for Hg(2+) ions that was simply prepared by micellar free radical polymerization of a water-insoluble organic rhodamine-based Hg(2+)-recognizing monomer (GR6GH), with hydrophilic monomers acrylamide (AM) and acrylic acid (AA). The chemical structure of the polymeric sensor was characterized by FT-IR and (1)H NMR spectroscopy. The apparent viscosity average molecular weight Mη of poly(acrylamide-acrylic acid) [poly(AM-NaAA)] and the water-soluble polymeric chemosensor poly(AM-NaAA-GR6GH) were 1.76 × 10(6) and 6.84 × 10(4) g/mol, respectively. Because of its amphiphilic property, the water-soluble polymeric chemosensor can be used as a chemosensor in aqueous media. Upon addition of Hg(2+) ions to an aqueous solution of poly(AM-NaAA-GR6GH), fluorescence enhancements were observed instantly. Moreover, other metal ions did not induce obvious changes to the fluorescence spectra. This approach may provide an easily measurable and inherently sensitive method for Hg(2+) ion detection in environmental and biological applications. PMID:25808221

  3. New Compstatin Peptides Containing N-Terminal Extensions and Non-Natural Amino Acids Exhibit Potent Complement Inhibition and Improved Solubility Characteristics

    PubMed Central

    2015-01-01

    Compstatin peptides are complement inhibitors that bind and inhibit cleavage of complement C3. Peptide binding is enhanced by hydrophobic interactions; however, poor solubility promotes aggregation in aqueous environments. We have designed new compstatin peptides derived from the W4A9 sequence (Ac-ICVWQDWGAHRCT-NH2, cyclized between C2 and C12), based on structural, computational, and experimental studies. Furthermore, we developed and utilized a computational framework for the design of peptides containing non-natural amino acids. These new compstatin peptides contain polar N-terminal extensions and non-natural amino acid substitutions at positions 4 and 9. Peptides with α-modified non-natural alanine analogs at position 9, as well as peptides containing only N-terminal polar extensions, exhibited similar activity compared to W4A9, as quantified via ELISA, hemolytic, and cell-based assays, and showed improved solubility, as measured by UV absorbance and reverse-phase HPLC experiments. Because of their potency and solubility, these peptides are promising candidates for therapeutic development in numerous complement-mediated diseases. PMID:25494040

  4. Discovery of a potent microtubule-targeting agent: Synthesis and biological evaluation of water-soluble amino acid prodrug of combretastatin A-4 derivatives.

    PubMed

    Yu, Kun; Li, Rong; Yang, Zhuang; Wang, Fang; Wu, Wenshuang; Wang, Xiaoyan; Nie, Chunlai; Chen, Lijuan

    2015-06-01

    Amino acid prodrugs are known to be very useful for improving the aqueous solubility of sparingly water soluble drugs (Drug Discovery Today 2013, 18, 93). Therefore, we synthesized eleven novel combretastatin A-4 amino acid derivatives and evaluated their anti-tumor activities in vitro and in vivo. Among them, compound 15 (valine attached to compound 3, which was shown to be a potent tubulin polymerization inhibitor in our previous study) exhibited high efficacy in tumor-bearing mice, and pharmacokinetic analysis in rats indicated that compound 15 was an effective prodrug as well. Besides, compound 15 significantly inhibited tubulin polymerization in vitro and in vivo by binding to the colchicine binding site. In addition, compound 15 induced cell cycle arrest in the G2/M phase and triggered apoptosis in a caspase-dependent manner. In conclusion, our study showed that compound 15 could have significant anti-tumor activity as a novel microtubule polymerization disrupting agent with improved aqueous solubility. PMID:25933592

  5. Solid microcrystalline dispersion films as a new strategy to improve the dissolution rate of poorly water soluble drugs: A case study using olanzapine.

    PubMed

    Modica de Mohac, Laura; de Fátima Pina, Maria; Raimi-Abraham, Bahijja Tolulope

    2016-07-11

    In this study, we evaluate the dissolution rate enhancement of solid microcrystalline dispersion (SMD) films of olanzapine (OLZ) formulated with four water-soluble polymers namely poly(N-vinylpyrrolidone) (PVP), poloxamer 188 (P188), poloxamer 407 (P407) and Soluplus(®) (SLP). Prepared formulations were characterised to determine particle size, morphology, hydrogen bonding interactions, thermal characteristics as well as in vitro dissolution studies conducted under sink conditions (pH 6.8). Particle size of OLZ in all formulations ranged between 42 and 58μm. Attenuated Total Reflectance Fourier Transform Infrared spectroscopy (ATR-FTIR), Differential Scanning Calorimetry (DSC) and Hot-Stage Microscopy (HSM) studies confirmed OLZ was well maintained in its crystalline state during the formulation process. In vitro dissolution studies showed immediate drug release from all formulation when compared to the drug alone. The greatest increase in in vitro dissolution rate was observed in formulations containing P188 most likely due to its enhanced hydrophilic and surfactant properties compared to the other agents used. Overall, this study successfully generated OLZ loaded SMD films with improved in vitro dissolution rates which is highly likely to result in improved oral bioavailability in vivo. PMID:27154255

  6. Evaluation of enzyme activity and fiber content of soybean cotyledon fiber and distiller's dried grains with solubles by solid state fermentation.

    PubMed

    Yang, Shengli; Lio, JunYi; Wang, Tong

    2012-05-01

    To increase the value of coproducts from corn ethanol fermentation and soybean aqueous processing, distiller's dried grains with solubles (DDGS) and soybean cotyledon fiber were used as the substrates for solid state fermentation (SSF) to improve feed digestibility. Aspergillus oryzae, Trichoderma reesei, and Phanerochaete chrysosporium were chosen as they produce desirable enzymes and are widely used in SSF for feed. The results showed that the cellulase and xylanase activities were significantly increased after 7 days of fermentation, and cellulose and hemicellulose degradation was also greatly increased. When soybean fiber was used as SSF substrate, the maximum activities of the cellulase and xylanase were 10.3 and 84.2 IU/g substrate (dry weight basis) after SSF treatment, respectively. However, the enzyme activities were relatively low in DDGS, and the growth of the three fungi was poor. The fungi grew better when soybean cotyledon fiber was added to DDGS, and cellulase and xylanase activity increased with the increase of soybean fiber content. Porosity was identified as an important factor for SSF because the addition of inert soybean hull alone improved the fungi growth significantly. These data suggest that the nutritional value of DDGS and soybean cotyledon fiber as monogastric animal feed could be greatly enhanced by SSF treatment. PMID:22528656

  7. A novel flow battery-A lead-acid battery based on an electrolyte with soluble lead(II). Part VI. Studies of the lead dioxide positive electrode

    NASA Astrophysics Data System (ADS)

    Pletcher, Derek; Zhou, Hantao; Kear, Gareth; Low, C. T. John; Walsh, Frank C.; Wills, Richard G. A.

    The structure of thick lead dioxide deposits (approximately 1 mm) formed in conditions likely to be met at the positive electrode during the charge/discharge cycling of a soluble lead-acid flow battery is examined. Compact and well adherent layers are possible with current densities >100 mA cm -2 in electrolytes containing 0.1-1.5 M lead(II) and methanesulfonic acid concentrations in the range 0-2.4 M; the solutions also contained 5 mM hexadecyltrimethylammonium cation, C 16H 33(CH 3) 3N +. From the viewpoint of the layer properties, the limitation is stress within the deposit leading to cracking and lifting away from the substrate; the stress appears highest at high acid concentration and high current density. There are, however, other factors limiting the maximum current density for lead dioxide deposition, namely oxygen evolution and the overpotential associated with the deposition of lead dioxide. A strategy for operating the soluble lead-acid flow battery is proposed.

  8. Long-term observation of water-soluble chemical components and acid-digested metals in the total suspended particles collected at Okinawa, Japan

    NASA Astrophysics Data System (ADS)

    Handa, D.; Okada, K.; Kuroki, Y.; Nakama, Y.; Nakajima, H.; Somada, Y.; Ijyu, M.; Azechi, S.; Oshiro, Y.; Nakaema, F.; Miyagi, Y.; Arakaki, T.; Tanahara, A.

    2011-12-01

    The economic growth and population increase in recent Asia have been increasing air pollution. Emission rate of air pollutants from Asia, in particular oxides of nitrogen, surpassed those from North America and Europe and should continue to exceed them for decades. Okinawa Island is situated approximately 1500 km south of Tokyo, Japan, 2000 km southeast of Beijing, China, and 1000 km south of South Korea. Its location is ideal in observing East Asia's air quality because maritime air mass prevails during summer, while continental air mass dominates during fall, winter, and spring. The maritime air mass data can be seen as background clean air and can be compared with continental air masses which have been affected by anthropogenic activities. We collected total suspended particles (TSP) on quartz filters by using a high volume air sampler at the Cape Hedo Atmosphere and Aerosol Monitoring Station (CHAAMS), Okinawa, Japan during August 2005 and August 2010. Sampling duration was one week for each sample. We determined the concentrations of water-soluble anions, cations, water-soluble organic carbon (WSOC) and acid-digested metals in TSP samples using ion chromatography, atomic absorption spectrometry, total organic carbon analyzer and Inductively Coupled Plasma Mass spectrometry (ICP-MS), respectively. Seasonal variation of water-soluble chemical components and acid-digested metals showed that the concentrations were the lowest in summer, higher in fall and winter, and the highest in spring. When air mass came from Asian continent, the concentrations of water-soluble chemical components and acid-digested metals were much higher compared to the other directions, suggesting long-range transport of air pollutants from Asian continent. Also, when the air mass came from Asian continent (75-100% dominant), the mean concentrations of non-sea salt sulfate and nitrate increased ca. 1.8 times and ca. 3.7 times, respectively between 2005 and 2010, and the ratio of nitrate to

  9. Solid phase extraction of petroleum carboxylic acids using a functionalized alumina as stationary phase.

    PubMed

    de Conto, Juliana Faccin; Nascimento, Juciara dos Santos; de Souza, Driele Maiara Borges; da Costa, Luiz Pereira; Egues, Silvia Maria da Silva; Freitas, Lisiane Dos Santos; Benvenutti, Edilson Valmir

    2012-04-01

    Petroleum essentially consists of a mixture of organic compounds, mainly containing carbon and hydrogen, and, in minor quantities, compounds with nitrogen, sulphur, and oxygen. Some of these compounds, such as naphthenic acids, can cause corrosion in pipes and equipment used in processing plants. Considering that the methods of separation or clean up the target compounds in low concentrations and in complex matrix use large amounts of solvents or stationary phases, is necessary to study new methodologies that consume smaller amounts of solvent and stationary phases to identify the acid components present in complex matrix, such as crude oil samples. The proposed study aimed to recover acid compounds using the solid phase extraction method, employing different types of commercial stationary ion exchange phases (SAX and NH(2)) and new phase alumina functionalized with 1,4-bis(n-propyl)diazoniabicyclo[2.2.2]octane chloride silsesquioxane (Dab-Al(2)O(3)), synthesized in this work. Carboxylic acids were used as standard mixture in the solid phase extraction for further calculation of recovery yield. Then, the real sample (petroleum) was fractionated into saturates, aromatics, resins, and asphaltenes, and the resin fraction of petroleum (B1) was eluted through stationary ion exchange phases. The stationary phase synthesized in this work showed an efficiency of ion exchange comparable to that of the commercial stationary phases. PMID:22589166

  10. Evaluation of soluble fraction and enzymatic residual fraction of dilute dry acid, ethylenediamine, and steam explosion pretreated corn stover on the enzymatic hydrolysis of cellulose.

    PubMed

    Qin, Lei; Liu, Li; Li, Wen-Chao; Zhu, Jia-Qing; Li, Bing-Zhi; Yuan, Ying-Jin

    2016-06-01

    This study is aimed to examine the inhibition of soluble fraction (SF) and enzymatic residual fraction (ERF) in dry dilute acid (DDA), ethylenediamine (EDA) and steam explosion (SE) pretreated corn stover (CS) on the enzymatic digestibility of cellulose. SF of DDA, EDA and SE pretreated CS has high xylose, soluble lignin and xylo-oligomer content, respectively. SF of EDA pretreated CS leads to the highest inhibition, followed by SE and DDA pretreated CS. Inhibition of ERF of DDA and SE pretreated CS is higher than that of EDA pretreated CS. The inhibition degree (A0/A) of SF is 1.76 and 1.21 times to that of ERF for EDA and SE pretreated CS, respectively. The inhibition degree of ERF is 1.05 times to that of SF in DDA pretreated CS. The quantitative analysis shows that SF of EDA pretreated CS, SF and ERF of SE pretreated CS cause significant inhibition during enzymatic hydrolysis. PMID:26970919

  11. Solid-phase synthesis of graphene quantum dots from the food additive citric acid under microwave irradiation and their use in live-cell imaging.

    PubMed

    Zhuang, Qianfen; Wang, Yong; Ni, Yongnian

    2016-05-01

    The work demonstrated that solid citric acid, one of the most common food additives, can be converted to graphene quantum dots (GQDs) under microwave heating. The as-prepared GQDs were further characterized by various analytical techniques like transmission electron microscopy, atomic force microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, fluorescence and UV-visible spectroscopy. Cytotoxicity of the GQDs was evaluated using HeLa cells. The result showed that the GQDs almost did not exhibit cytotoxicity at concentrations as high as 1000 µg mL(-1) . In addition, it was found that the GQDs showed good solubility, excellent photostability, and excitation-dependent multicolor photoluminescence. Subsequently, the multicolor GQDs were successfully used as a fluorescence light-up probe for live-cell imaging. Copyright © 2015 John Wiley & Sons, Ltd. PMID:26310294

  12. Nano-tribological and wear behavior of boric acid solid lubricant.

    SciTech Connect

    Mirmiran, S.; Tsukruk, V. V.; Erdemir, A.; Energy Technology; Western Michigan Univ.

    1999-01-01

    One uses atomic force microscopy to explore the surface morphology, frictional characteristics (i.e., friction mapping) and surface adhesive forces of boric acid-treated aluminum surfaces. In earlier studies, boric acid was shown to be an effective solid lubricant providing 0.02 to 0.1 friction coefficients to the sliding surfaces of metallic and ceramic materials. In this study, the authors mainly focused on the friction and wear behavior of cleaved single crystals of boric acid. Tests were performed on uncoated and boric acid-coated surfaces of aluminum substrates, as well as the bulk boric acid material. The nano-scale wear of the boric acid crystals manifested itself in the displacement of atomic planes which, in turn, resulted in the formation of the worn area grown by a spiral-growth mechanism. In addition, new crystals in the vicinity of the sliding contact areas were formed. These crystals formed by a spiral dislocation mechanism. The nanoscale friction measurements showed that the friction coefficient of a Si{sub 3}N{sub 4} tip against the boric acid single crystal, was in the range of 0.07 to 0.13, depending on the sliding direction with respect to the crystallographic orientation. The friction coefficients of the boric acid-coated aluminum substrates varied between 0.11 and 0.19. While these values were consistent with earlier findings and further demonstrated the lubricity of boric acid, they were higher than the previous measurements (i.e., 0.011-0.1) obtained on a pin-on-disk machine using steel or ceramic pins. An explanation is provided for this phenomenon.

  13. Relationship between the solubility, dosage and antioxidant capacity of carnosic acid in raw and cooked ground buffalo meat patties and chicken patties.

    PubMed

    Naveena, B M; Vaithiyanathan, S; Muthukumar, M; Sen, A R; Kumar, Y Praveen; Kiran, M; Shaju, V A; Chandran, K Ramesh

    2013-10-01

    Antioxidant capacity of oil soluble and water dispersible carnosic acid (CA) extracted from dried rosemary leaves using HPLC was evaluated at two different dosages (22.5 ppm vs 130 ppm) in raw and cooked ground buffalo meat patties and chicken patties. Irrespective of total phenolic content, CA extracts reduced (p<0.05) the thiobarbituric acid reactive substances (TBARS) by 39%-47% and 37%-40% in cooked buffalo meat and chicken patties at lower dosage (22.5 ppm) relative to control samples. However, at higher dosage (130 ppm) the TBARS values were reduced (p<0.05) by 86%-96% and 78%-87% in cooked buffalo meat and chicken patties compared to controls. The CA extracts were also effective in inhibiting (p<0.05) peroxide value and free fatty acids in cooked buffalo meat and chicken patties. The CA extracts when used at higher dosage, were also effective in stabilizing raw buffalo meat color. PMID:23743029

  14. [Acid-soluble collagen in the skin of rats who received a tryptophan load and were kept on a protein-free diet].

    PubMed

    Pechenova, T N; Gulyĭ, M F; Volodina, T T; Solodova, E V; Popova, N N

    1983-01-01

    Crystalline preparations of acid-soluble collagen of rat skin in norm and with tryptophan load against a background of the protein-free diet were fractionated by differential salting out using NaCl in concentrations corresponding to precipitation zones of collagen 1,3 and 4. Amino acid composition, electrophoretic mobility in polyacrylamide gel, profiles of elution from CM-cellulose, content of the carbohydrate component and--S--S-bonds were studied in proteins of the mentioned fractions and in the precipitate insoluble after the pepsin action. Essential differences as compared to the normal level in the amino acid composition and elution profiles were detected in the fraction corresponding to collagen I. Quantitative changes in the carbohydrate component and--S--S-bonds occur due to the fraction inaccessible to the persin action. PMID:6829075

  15. Preparation of water-soluble hyperbranched polyester nanoparticles with sulfonic acid functional groups and their micelles behavior, anticoagulant effect and cytotoxicity.

    PubMed

    Han, Qiaorong; Chen, Xiaohan; Niu, Yanlian; Zhao, Bo; Wang, Bingxiang; Mao, Chun; Chen, Libin; Shen, Jian

    2013-07-01

    Biocompatibility of nanoparticles has been attracting great interest in the development of nanoscience and nanotechnology. Herein, the aliphatic water-soluble hyperbranched polyester nanoparticles with sulfonic acid functional groups (HBPE-SO3 NPs) were synthesized and characterized. They are amphiphilic polymeric nanoparticles with hydrophobic hyperbranched polyester (HBPE) core and hydrophilic sulfonic acid terminal groups. Based on our observations, we believe there are two forms of HBPE-SO3 NPs in water under different conditions: unimolecular micelles and large multimolecular micelles. The biocompatibility and anticoagulant effect of the HBPE-SO3 NPs were investigated using coagulation tests, hemolysis assay, morphological changes of red blood cells (RBCs), complement and platelet activation detection, and cytotoxicity (MTT). The results confirmed that the sulfonic acid terminal groups can substantially enhance the anticoagulant property of HBPE, and the HBPE-SO3 NPs have the potential to be used in nanomedicine due to their good bioproperties. PMID:23718279

  16. Fatty acids for controlled release applications: A comparison between prilling and solid lipid extrusion as manufacturing techniques.

    PubMed

    Vervaeck, A; Monteyne, T; Siepmann, F; Boone, M N; Van Hoorebeke, L; De Beer, T; Siepmann, J; Remon, J P; Vervaet, C

    2015-11-01

    The aim of the present study was to evaluate the solid state characteristics, drug release and stability of fatty acid-based formulations after processing via prilling and solid lipid extrusion. Myristic acid (MA), stearic acid (SA) and behenic acid (BA) were used as matrix formers combined with metoprolol tartrate (MPT) as model drug. The prilling process allowed complete dissolution of MPT in the molten fatty acid phase, generating semi-crystalline MPT and the formation of hydrogen bonds between drug and fatty acids in the solid prills. In contrast, as solid lipid extrusion (SLE) induced only limited melting of the fatty acids, molecular interaction with the drug was inhibited, yielding crystalline MPT. Although the addition of a low melting fatty acid allowed more MPT/fatty acid interaction during extrusion, crystalline MPT was detected after processing. Mathematical modeling revealed that the extrudates exhibited a higher apparent drug/water mobility than prills of the same composition, probably due to differences in the inner systems' structure. Irrespective of the processing method, mixed fatty acid systems (e.g. MA/BA) exhibited a lower matrix porosity, resulting in a slower drug release rate. Solid state analysis of these systems indicated that the crystalline structure of the fatty acids was maintained after SLE, while prilling generated a reduced MA crystallinity. Binary MPT/fatty acid systems processed via extrusion showed better stability during storage at 40 °C than the corresponding prills. Although mixed fatty acid systems were stable at 25 °C, stability problems were encountered during storage at 40 °C: a faster release was obtained from the prills, whereas drug release from the extrudates was slower. PMID:26428938

  17. α-Azido Acids in Solid-Phase Peptide Synthesis: Compatibility with Fmoc Chemistry and an Alternative Approach to the Solid Phase Synthesis of Daptomycin Analogs.

    PubMed

    Lohani, Chuda Raj; Rasera, Benjamin; Scott, Bradley; Palmer, Michael; Taylor, Scott D

    2016-03-18

    α-Azido acids have been used in solid phase peptide synthesis (SPPS) for almost 20 years. Here we report that peptides bearing an N-terminal α-azidoaspartate residue undergo elimination of an azide ion when treated with reagents that are commonly used for removing the Fmoc group during SPPS. We also report an alternative solid-phase route to the synthesis of an analog of daptomycin that uses a reduced number of α-azido amino acids and without elimination of an azide ion. PMID:26938305

  18. Ethyl oleate-containing nanostructured lipid carriers improve oral bioavailability of trans-ferulic acid ascompared with conventional solid lipid nanoparticles.

    PubMed

    Zhang, Yongtai; Li, Zhe; Zhang, Kai; Yang, Gang; Wang, Zhi; Zhao, Jihui; Hu, Rongfeng; Feng, Nianping

    2016-09-10

    trans-Ferulic acid (TFA) has antioxidative, anti-inflammatory, and cardioprotective effects, but its poor solubility in water results in unsatisfactory oral bioavailability when administered conventionally at a standard dosage. However, the limited bioavailability of TFA can be overcome by delivering it in nanostructured lipid carriers (NLCs). In this study, a microemulsion (ME)-based method was used to prepare NLCs with ethyl oleate as the liquid lipid component and glyceryl behenate as the solid lipid component. These NLCs and solid lipid nanoparticles (SLNs) were then used as vehicles for TFA. Their entrapment efficiencies (EE), stability during storage, in vitro release profiles, and in vivo pharmacokinetics were compared. The NLC formulation afforded a drug entrapment efficiency that was significantly greater than that of the SLN formulation, which was made using a single solid lipid. Furthermore, the TFA that was dispersed in the disordered binary lipid matrix of the NLC formulation was more stable than that in the SLN formulation, and thus showed less expulsion from the vehicle during storage. In in vivo pharmacokinetic studies, the NLC TFA formulation yielded a greater Cmax and AUC than that produced by the SLN formulation and an aqueous TFA suspension. This showed that the oral bioavailability of TFA was markedly improved by packaging in NLCs. NLCs are thus a promising vehicle for oral TFA administration, with significant advantages over SLNs. PMID:27374194

  19. Variability, formation and acidity of water-soluble ions in PM2.5 in Beijing based on the semi-continuous observations

    NASA Astrophysics Data System (ADS)

    Hu, Guoyuan; Zhang, Yangmei; Sun, Junying; Zhang, Leiming; Shen, Xiaojing; Lin, Weili; Yang, Yun

    2014-08-01

    Daily PM2.5 and hourly water-soluble inorganic ions in PM2.5 and gaseous precursors were measured during June-November 2009 at an urban site in Beijing. The average mass concentration of the total water-soluble ions was 44 μg m- 3, accounting for 38% of PM2.5. Sulfate (SO42 -), nitrate (NO3-) and ammonium (NH4+) were dominant ions. The summer-fall difference in seasonal average mass concentrations was smaller than 30% for SO42 -, but was up to a factor of 2.0 for NO3- and NH4+. A pronounced diurnal cycle was found for most ions and gaseous precursors and could be explained by their respective sources, formation mechanisms and meteorological conditions. The average oxidation/conversion ratio for SO42 - (SOR), NO3- (NOR) and NH4+ (NHR) were estimated to be 63%, 15% and 15%, respectively. The low NHR value suggests that NH3 was mainly from local sources and that excessive NH3 existed and thus was not a limiting factor in the formation of NH4+. As a result, the diurnal pattern of NH4+ was similar to that of SO42 - to some extent, but differed significantly from that of NH3. Based on the estimated H+ concentration and acidity purity (f), 75% of data samples were strongly acidic and a few percent might be alkaline. Seasonal variations in aerosol acidity and chemical forms of major ions were also briefly discussed.

  20. Efficiency of buffered aqueous carboxylic acid solutions and organic solvents to absorb SO/sub 2/ from industrial flue gas; solubility data from gas-liquid chromatography

    SciTech Connect

    Sanza, G.J.

    1982-01-01

    Nine adsorbents were examined. These potential candidates for flue gas desulfurization included 1-methyl-2-pyrrolidinone, tri-n-butyl phosphate (TBP), both 0.5 M and 1.0 M solutions of citric acid and glycolic acid, buffered to pH's of 4.5 and 3.8, and pure water. Infinite dilution activity coefficients of SO/sub 2/ were obtained by gas-liquid chromatography in a trial solvent of Nitrobenzene, and then in systems of 1-methyl-2-pyrrolidinone and TBP, independently. The solubility data of SO/sub 2/ was derived and found to be comparable to data obtained from a classical bubble-sparger apparatus. Solubility data was then programmed into an absorber-stripper computer simulator in order to calculate the various concentration and temperature profiles that would exist, the degree of desulfurization, and the steam consumption for all nine systems. Concentrated solutions of citric acid buffered to a low pH exhibited the most favorable conditions for application in direct steam regeneration processes. 1-methyl-2-pyrrolidinone yielded better performance than TBP did with high-pressure indirect steam used for stripping. Comparison between the aqueous solution systems which employed direct steam, and the organic systems which used indirect steam was inconclusive.

  1. Solid-Phase Formation Of Isovaline, A Non-Biological, Meteoritic Amino Acid

    NASA Astrophysics Data System (ADS)

    Hudson, Reggie L.; Lewis, A. S.; Moore, M. H.; Dworkin, J. P.; Glavin, D. P.

    2007-10-01

    Among the Murchison (CM) meteoritic amino acids, isovaline stands out as being non-biological (nonprotein) and having a high abundance. Approximately equal amounts of D- and L-isovaline have been reported in CM meteorites, but the molecule's structure appears to prohibit racemization in aqueous solutions. While it is possible that isovaline could be made by the oft-studied Strecker reaction, laboratory experiments have seldom been able to produce this molecule from realistic molecular precursors. Recently we have investigated the low-temperature solid-phase chemistry of isovaline with an eye toward the molecule's formation, its stability, and the interconversion of its D- and L-enantiomers. Ion-irradiated isovaline-containing ices were examined by IR spectroscopy and highly-sensitive LC/ToF-MS methods to assess both amino acid destruction and racemization. Samples were studied both in the presence and absence of water-ice, and the destruction of isovaline was measured as a function of radiation dose. In addition, we have continued our earlier work on solid-phase amino acid formation, extending it to cover isovaline. In this presentation we will report the results of these newer investigations. This work was supported by a grant to the Goddard Center for Astrobiology through the NASA Astrobiology Institute. AL was supported by an award from the Summer Undergraduate Internship in Astrobiology program.

  2. Bacterial dynamics and metabolite changes in solid-state acetic acid fermentation of Shanxi aged vinegar.

    PubMed

    Li, Sha; Li, Pan; Liu, Xiong; Luo, Lixin; Lin, Weifeng

    2016-05-01

    Solid-state acetic acid fermentation (AAF), a natural or semi-controlled fermentation process driven by reproducible microbial communities, is an important technique to produce traditional Chinese cereal vinegars. Highly complex microbial communities and metabolites are involved in traditional Chinese solid-state AAF, but the association between microbiota and metabolites during this process are still poorly understood. In this study, we performed amplicon 16S rRNA gene sequencing on the Illumina MiSeq platform, PCR-denaturing gradient gel electrophoresis, and metabolite analysis to trace the bacterial dynamics and metabolite changes under AAF process. A succession of bacterial assemblages was observed during the AAF process. Lactobacillales dominated all the stages. However, Acetobacter species in Rhodospirillales were considerably accelerated during AAF until the end of fermentation. Quantitative PCR results indicated that the biomass of total bacteria showed a "system microbe self-domestication" process in the first 3 days, and then peaked at the seventh day before gradually decreasing until the end of AAF. Moreover, a total of 88 metabolites, including 8 organic acids, 16 free amino acids, and 66 aroma compounds were detected during AAF. Principal component analysis and cluster analyses revealed the high correlation between the dynamics of bacterial community and metabolites. PMID:26754813

  3. Protein solubility modeling

    NASA Technical Reports Server (NTRS)

    Agena, S. M.; Pusey, M. L.; Bogle, I. D.

    1999-01-01

    A thermodynamic framework (UNIQUAC model with temperature dependent parameters) is applied to model the salt-induced protein crystallization equilibrium, i.e., protein solubility. The framework introduces a term for the solubility product describing protein transfer between the liquid and solid phase and a term for the solution behavior describing deviation from ideal solution. Protein solubility is modeled as a function of salt concentration and temperature for a four-component system consisting of a protein, pseudo solvent (water and buffer), cation, and anion (salt). Two different systems, lysozyme with sodium chloride and concanavalin A with ammonium sulfate, are investigated. Comparison of the modeled and experimental protein solubility data results in an average root mean square deviation of 5.8%, demonstrating that the model closely follows the experimental behavior. Model calculations and model parameters are reviewed to examine the model and protein crystallization process. Copyright 1999 John Wiley & Sons, Inc.

  4. Gold solubility and partitioning between sulfide liquid, monosulfide solid solution and hydrous mantle melts: Implications for the formation of Au-rich magmas and crust-mantle differentiation

    NASA Astrophysics Data System (ADS)

    Li, Yuan; Audétat, Andreas

    2013-10-01

    The solubility of Au in sulfur-free vs. sulfide-saturated melts and its partitioning behavior between sulfide liquid (SL), monosulfide solid solution (MSS) and hydrous basanite melt at variable Au activities was investigated in a fO2 range of FMQ-2 to FMQ+1.6 at 1200 °C/1.5 GPa using piston cylinder apparatus. Gold solubility in sulfur-free (<100 μg/g S) melt is low (0.6-1.6 μg/g) and increases with fO2 in a manner consistent with Au dissolution as AuO1/2, whereas in sulfide-saturated melts it is high (13.6 ± 1.7 μg/g) and independent of fO2. Variations in the chlorine content of sulfide-saturated melts (0.2-1.2 wt% Cl) had no measurable effect on Au solubility. Gold partition coefficients between sulfide liquid and silicate melt (DAuSL/SM) are very high, ∼10,000 ± 3000, which is at the upper end of values reported in previous studies. Gold partition coefficients between MSS and silicate melt (DAuMSS/SM) are much lower, 60 ± 10, which is at the lower end of previous values. Both DAuSL/SM and DAuMSS/SM are independent of fO2. The new Au partition coefficients were used in conjunction with previously published Cu and Ag partition coefficients to investigate the role of MSS versus SL during partial melting in the source region of primitive potassic magmas and during crust-mantle differentiation. The high Au content of ore deposits associated with potassic magmas has commonly been explained by the dissolution of Au-rich sulfide liquid, either during partial melting in the mantle source or during partial re-melting of sulfide-bearing cumulates at the crust-mantle boundary. We argue that MSS is the dominant sulfide phase in the mantle source region of these magmas, and thus that their high Au content is a consequence of low MSS-silicate melt partition coefficients rather than of sulfide exhaustion or partial re-melting of sulfide-bearing cumulates. Continental crust is depleted in Au, Ag and Cu relative to mantle melts, which was thought to be due to removal of

  5. Solid-state fermentation for gluconic acid production from sugarcane molasses by Aspergillus niger ARNU-4 employing tea waste as the novel solid support.

    PubMed

    Sharma, Amit; Vivekanand, V; Singh, Rajesh P

    2008-06-01

    Solid-state fermentation (SSF) was evaluated to produce gluconic acid by metal resistant Aspergillus niger (ARNU-4) strain using tea waste as solid support and with molasses based fermentation medium. Various crucial parameters such as moisture content, temperature, aeration and inoculum size were derived; 70% moisture level, 30 degrees C temperature, 3% inoculum size and an aeration volume of 2.5l min(-1) was suited for maximal (76.3 gl(-1)) gluconic acid production. Non-clarified molasses based fermentation media was utilized by strain ARNU-4 and maximum gluconic acid production was observed following 8-12 days of fermentation cycle. Different concentrations of additives viz. oil cake, soya oil, jaggary, yeast extract, cheese whey and mustard oil were supplemented for further enhancement of the production ability of microorganism. Addition of yeast extract (0.5%) was observed inducive for enhanced (82.2 gl(-1)) gluconic acid production. PMID:17881224

  6. Synthesis of sulfonated porous carbon nanospheres solid acid by a facile chemical activation route

    NASA Astrophysics Data System (ADS)

    Chang, Binbin; Guo, Yanzhen; Yin, Hang; Zhang, Shouren; Yang, Baocheng

    2015-01-01

    Generally, porous carbon nanospheres materials are usually prepared via a template method, which is a multi-steps and high-cost strategy. Here, we reported a porous carbon nanosphere solid acid with high surface area and superior porosity, as well as uniform nanospheical morphology, which prepared by a facile chemical activation with ZnCl2 using resorcinol-formaldehyde (RF) resins spheres as precursor. The activation of RF resins spheres by ZnCl2 at 400 °C brought high surface area and large volume, and simultaneously retained numerous oxygen-containing and hydrogen-containing groups due to the relatively low processing temperature. The presence of these functional groups is favorable for the modification of -SO3H groups by a followed sulfonation treating with sulphuric acid and organic sulfonic acid. The results of N2 adsorption-desorption and electron microscopy clearly showed the preservation of porous structure and nanospherical morphology. Infrared spectra certified the variation of surface functional groups after activation and the successful modification of -SO3H groups after sulfonation. The acidities of catalysts were estimated by an indirect titration method and the modified amount of -SO3H groups were examined by energy dispersive spectra. The results suggested sulfonated porous carbon nanospheres catalysts possessed high acidities and -SO3H densities, which endowed their significantly catalytic activities for biodiesel production. Furthermore, their excellent stability and recycling property were also demonstrated by five consecutive cycles.

  7. Coke-free direct formic acid solid oxide fuel cells operating at intermediate temperatures

    NASA Astrophysics Data System (ADS)

    Chen, Yubo; Su, Chao; Zheng, Tao; Shao, Zongping

    2012-12-01

    Formic acid is investigated as a fuel for Solid Oxide Fuel Cells (SOFCs) for the first time. Thermodynamic calculations demonstrate that carbon deposition is avoidable above 600 °C. The carbon deposition properties are also investigated experimentally by first treating a nickel plus yttria-stabilized zirconia (Ni-YSZ) anode material in particle form under a formic acid-containing atmosphere for a limited time at 500-800 °C and then analyzing the particles by O2-TPO. This analysis confirms that carbon deposition on Ni-YSZ is weak above 600 °C. We further treat half-cells composed of YSZ electrolyte and Ni-YSZ anode under formic acid-containing atmosphere at 600, 700 and 800 °C; the anodes maintain their original geometric shape and microstructure and show no obvious weight gain. It suggests that formic acid can be directly fed into SOFCs constructed with conventional nickel-based cermet anodes. I-V tests show that the cell delivers a promising peak power density of 571 mW cm-2 at 800 °C. In addition, the cells also show good performance stability. The results indicate that formic acid is highly promising as a direct fuel for SOFCs without the need for cell material modifications.

  8. Towards an understanding of the molecular mechanism of solvation of drug molecules: a thermodynamic approach by crystal lattice energy, sublimation, and solubility exemplified by hydroxybenzoic acids.

    PubMed

    Perlovich, German L; Volkova, Tatyana V; Bauer-Brandl, Annette

    2006-07-01

    Temperature dependencies of saturated vapor pressure and heat capacities for the 2-, 3-, and 4-hydroxybenzoic acids were measured and thermodynamic functions of sublimation calculated (2-hydroxybenzoic acid: DeltaG(sub) (298) = 38.5 kJ/mol; DeltaH(sub) (298) = 96.6 +/- 0.8 kJ/mol; DeltaS(sub) (298) = 191 +/- 3 J/mol . K; 3-hydroxybenzoic acid: DeltaG(sub) (298) = 50.6 kJ/mol; DeltaH(sub) (298) = 105.2 +/- 0.8 kJ/mol; DeltaS(sub) (298) = 180 +/- 2 J/mol . K; 4-hydroxybenzoic acid: DeltaG(sub) (298) = 55.0 kJ/mol; DeltaH(sub) (298) = 113.3 +/- 0.7 kJ/mol; DeltaS(sub) (298) = 193 +/- 2 J/mol . K). Analysis of crystal lattice packing energies based on geometry optimization of the molecules in the crystal using diffraction data and the program Dmol(3) was carried out. The energetic contributions of van der Waals, Coulombic, and hydrogen bond terms to the total packing energy were analyzed. The fraction of hydrogen bond energy in the packing energy increases as: 3-hydroxybenzoic (29.7%) < 2-hydroxybenzoic (34.7%) < 4-hydroxybenzoic acid (42.0%). Enthalpies of evaporation were estimated from enthalpies of sublimation and fusion. Temperature dependencies of the solubility in n-octanol and n-hexane were measured. The thermodynamic functions of solubility and solvation processes were deduced. Specific and nonspecific solvation terms were distinguished using the transfer from the "inert" n-hexane to the other solvents. The transfer of the molecules from water to n-octanol is enthalpy driven process. PMID:16729271

  9. Preparation of a novel carbon-based solid acid from cassava stillage residue and its use for the esterification of free fatty acids in waste cooking oil.

    PubMed

    Wang, Lingtao; Dong, Xiuqin; Jiang, Haoxi; Li, Guiming; Zhang, Minhua

    2014-04-01

    A novel carbon-based solid acid catalyst was prepared by the sulfonation of incompletely carbonized cassava stillage residue (CSR) with concentrated sulfuric acid, and employed to catalyze the esterification of methanol and free fatty acids (FFAs) in waste cooking oil (WCO). The effects of the carbonization and the sulfonation temperatures on the pore structure, acid density and catalytic activity of the CSR-derived catalysts were systematically investigated. Low temperature carbonization and high temperature sulfonation can cause the collapse of the carbon framework, while high temperature carbonization is not conducive to the attachment of SO3H groups on the surface. The catalyst showed high catalytic activity for esterification, and the acid value for WCO is reduced to below 2mg KOH/g after reaction. The activity of catalyst can be well maintained after five cycles. CSR can be considered a promising raw material for the production of a new eco-friendly solid acid catalyst. PMID:24661813

  10. Soluble solids content and firmness non-destructive inspection and varieties discrimination of apples based on visible near-infrared hyperspectral imaging

    NASA Astrophysics Data System (ADS)

    Zhou, Yao

    2014-11-01

    For apples, soluble solids content (SSC) and firmness are two very important internal quality attributes, which play key roles in postharvest quality classification. Visible-near infrared hyper spectral imaging techniques have potentials for nondestructive inspection of apples' internal qualities, which will be used for the SSC and firmness non-destructive inspection and varieties discrimination of apples. Spectrums of 396 apples from four varieties were extracted. There were 264 apples used for calibration and the remaining 132 apples for prediction. After collecting hyper spectral images of calibration apples, the sugar meter and firmness tester was used to measure SSC and firmness's reference values of each calibration apples. Then the principal component analysis (PCA) was used to extract effective wavelengths of calibration apples. The reference values and effective wavelengths' reflectance of apples can be used to set linear regression models based on partial least squares (PLS). Once the prediction model was established, in order to get the SSC and firmness's predicted values of apples, it only need achieve the effective wavelengths' reflectance of apples combing with the program of MATLAB. Finally, the SSC and firmness values of prediction set were used as independent variables of the Linear Discriminant Analysis (LDA) to realize varieties discrimination. The correlation coefficients were 0.9127 for SSC and 0.9608 for firmness values of prediction models. The accuracy of varieties discrimination was 96.97%. The results indicated that the methods to SSC and firmness non-destructive inspection and varieties discrimination of apples based on Vis-NIR hyper spectral imaging was reliable and feasible.

  11. Biodegradable Poly (Lactic-co-Glycolic Acid)-Polyethylene Glycol Nanocapsules: An Efficient Carrier for Improved Solubility, Bioavailability, and Anticancer Property of Lutein.

    PubMed

    Arunkumar, Ranganathan; Prashanth, Keelara Veerappa Harish; Manabe, Yuki; Hirata, Takashi; Sugawara, Tatsuya; Dharmesh, Shylaja Mallaiah; Baskaran, Vallikannan

    2015-06-01

    Lutein bioavailability is limited because of its poor aqueous solubility. In this study, lutein-poly (lactic-co-glycolic acid) (PLGA)-polyethylene glycol (PEG) nanocapsules were prepared to improve the solubility, bioavailability, and anticancer property of lutein. The scanning electron microscopy and dynamic light scattering examination revealed that the nanocapsules are smooth and spherical with size ranging from 80 to 500 nm (mean = 200 nm). In vitro lutein release profile from nanocapsules showed controlled sustainable release (66%) up to 72 h. Aqueous solubility of lutein nanocapsules was much higher by 735-fold than the lutein. Fourier transform infrared spectroscopy analyses showed no chemical interaction among PLGA, PEG, and lutein, indicating possible weak intermolecular forces like hydrogen bonds. X-ray diffraction revealed lutein is distributed in a disordered amorphous state in nanocapsules. Postprandial plasma kinetics (area under the curve) of an oral dose of lutein from nanocapsules was higher by 5.4-fold compared with that of micellar lutein (control). The antiproliferative effect of lutein from nanocapsules (IC50 value, 10.9 μM) was higher (43.6%) than the lutein (IC50 value, 25 μM). Results suggest that PLGA-PEG nanocapsule is an efficient carrier for enhancing hydrophilicity, bioavailability, and anticancer property of lipophilic molecules such as lutein. PMID:25824524

  12. Solubility and modeling acid-base properties of adrenaline in NaCl aqueous solutions at different ionic strengths and temperatures.

    PubMed

    Bretti, Clemente; Cigala, Rosalia Maria; Crea, Francesco; De Stefano, Concetta; Vianelli, Giuseppina

    2015-10-12

    Solubility and acid-base properties of adrenaline were studied in NaCl aqueous solutions at different ionic strengths (0solubility of the ligand was calculated from simple mass balance equations, by using the free hydrogen concentration and the protonation constants of the ligand determined in the same experimental conditions of the solubility measurements. The salting-In or Out parameters and the activity coefficient of the neutral species were calculated by means of the Setschenow equation. The dependence of the protonation constants on the ionic strength was modeled by means of the Debye-Hückel type equation and of the SIT (Specific ion Interaction Theory) approach. The specific interaction parameters of the ion pairs were also reported. For the protonation constants, the following thermodynamic values at infinite dilution were obtained: T=298.15 K, logK1(H0)=10.674±0.018 and logK2(H0)=8.954±0.022; T=310.15K, logK1(H0)=10.355±0.018 and logK2(H0)=8.749±0.030. PMID:26122929

  13. Hyaluronic acid based self-assembling nanosystems for CD44 target mediated siRNA delivery to solid tumors

    PubMed Central

    Ganesh, Shanthi; Iyer, Arun K.; Morrissey, David V.; Amiji, Mansoor M.

    2013-01-01

    Anticancer therapeutics employing RNA interference mechanism holds promising potentials for sequence-specific silencing of target genes. However targeted delivery of siRNAs to tumor tissues and cells and more importantly, their intracellular release at sites of interest still remains a major challenge that needs to be addressed before this technique could become a clinically viable option. In the current study, we have engineered and screened a series of CD44 targeting hyaluronic acid (HA) based self-assembling nanosystems for targeted siRNA delivery. The HA polymer was functionalized with lipids of varying carbon chain lengths/nitrogen content, as well as polyamines for assessing siRNA encapsulation. From the screens, several HA-derivatives were identified that could stably encapsulate/complex siRNAs and form self-assembled nanosystems, as determined by gel retardation assays and dynamic light scattering. Many HA derivatives could transfect siRNAs into cancer cells overexpressing CD44 receptors. Interestingly, blocking the CD44 receptors on the cells using free excess soluble HA prior to incubation of cy3-labeled-siRNA loaded HA nano-assemblies resulted in >90% inhibition of the receptor mediated uptake, confirming target specificity. In addition, SSB/PLK1 siRNA encapsulated in HA-PEI/PEG nanosystems demonstrated dose dependent and target specific gene knockdown in both sensitive and resistant A549 lung cancer cells overexpressing CD44 receptors. More importantly, these siRNA encapsulated nanosystems demonstrated tumor selective uptake and target specific gene knock down in vivo in solid tumors as well as in metastatic tumors. The HA based nanosystems thus portend to be promising siRNA delivery vectors for systemic targeting of CD44 overexpressing cancers including tumor initiating (stem-) cells and metastatic lesions. PMID:23410679

  14. Ionic and Covalent Stabilization of Intermediates and Transition States in Catalysis by Solid Acids

    SciTech Connect

    Deshlahra, Prashant; Carr, Robert T.; Iglesia, Enrique

    2014-10-29

    Reactivity descriptors describe catalyst properties that determine the stability of kinetically relevant transition states and adsorbed intermediates. Theoretical descriptors, such as deprotonation energies (DPE), rigorously account for Brønsted acid strength for catalytic solids with known structure. Here, mechanistic interpretations of methanol dehydration turnover rates are used to assess how charge reorganization (covalency) and electrostatic interactions determine DPE and how such interactions are recovered when intermediates and transition states interact with the conjugate anion in W and Mo polyoxometalate (POM) clusters and gaseous mineral acids. Turnover rates are lower and kinetically relevant species are less stable on Mo than W POM clusters with similar acid strength, and such species are more stable on mineral acids than that predicted from W-POM DPE–reactivity trends, indicating that DPE and acid strength are essential but incomplete reactivity descriptors. Born–Haber thermochemical cycles indicate that these differences reflect more effective charge reorganization upon deprotonation of Mo than W POM clusters and the much weaker reorganization in mineral acids. Such covalency is disrupted upon deprotonation but cannot be recovered fully upon formation of ion pairs at transition states. Predictive descriptors of reactivity for general classes of acids thus require separate assessments of the covalent and ionic DPE components. Here, we describe methods to estimate electrostatic interactions, which, taken together with energies derived from density functional theory, give the covalent and ionic energy components of protons, intermediates, and transition states. In doing so, we provide a framework to predict the reactive properties of protons for chemical reactions mediated by ion-pair transition states.

  15. Solid-state NMR studies of theophylline co-crystals with dicarboxylic acids.

    PubMed

    Pindelska, Edyta; Sokal, Agnieszka; Szeleszczuk, Lukasz; Pisklak, Dariusz Maciej; Kolodziejski, Waclaw

    2014-11-01

    In this work, three polycrystalline materials containing co-crystals of theophylline with malonic, maleic, and glutaric acids were studied using (13)C, (15)N and (1)H solid-state NMR and FT-IR spectroscopy. The NMR assignments were supported by gauge including projector augmented waves (GIPAW) calculations of chemical shielding, performed using X-ray determined geometry. The experimental (13)C cross polarization/magic angle spinning (CP/MAS) NMR results and the calculated isotropic chemical shifts were in excellent agreement. A rapid and convenient method for theophylline co-crystals crystal structure analysis has been proposed for co-crystals, which are potentially new APIs. PMID:25194346

  16. Hydrochloric acid aerosol and gaseous hydrogen chloride partitioning in a cloud contaminated by solid rocket exhaust

    NASA Technical Reports Server (NTRS)

    Sebacher, D. I.; Bendura, R. J.; Wornom, D. E.

    1980-01-01

    Partitioning of hydrogen chloride between hydrochloric acid aerosol and gaseous HCl in the lower atmosphere was experimentally investigated in a solid rocket exhaust cloud diluted with humid ambient air. Airborne measurements were obtained of gaseous HCl, total HCl, relative humidity and temperature to evaluate the conditions under which aerosol formation occurs in the troposphere in the presence of hygroscopic HCl vapor. Equilibrium predictions of HCl aerosol formation accurately predict the measured HCl partitioning over a range of total HCl concentrations from 0.6 to 16 ppm.

  17. Determination of the mean solid-liquid interface energy of pivalic acid

    NASA Technical Reports Server (NTRS)

    Singh, N. B.; Gliksman, M. E.

    1989-01-01

    A high-confidence solid-liquid interfacial energy is determined for an anisotropic material. A coaxial composite having a cylindrical specimen chamber geometry provides a thermal gradient with an axial heating wire. The surface energy is derived from measurements of grain boundary groove shapes. Applying this method to pivalic acid, a surface energy of 2.84 erg/sq cm was determined with a total systematic and random error less than 10 percent. The value of interfacial energy corresponds to 24 percent of the latent heat of fusion per molecule.

  18. Synthesis of all nineteen appropriately protected chiral alpha-hydroxy acid equivalents of the alpha-amino acids for Boc solid-phase depsi-peptide synthesis.

    PubMed

    Deechongkit, Songpon; You, Shu-Li; Kelly, Jeffery W

    2004-02-19

    [reaction: see text] The preparation of depsi-peptides, amide-to-ester-substituted peptides used to probe the role of hydrogen bonding in protein folding energetics, is accomplished by replacing specific l-alpha-amino acid residues by their alpha-hydroxy acid counterparts in a solid-phase synthesis employing a t-Boc strategy. Herein we describe the efficient stereoselective synthesis of all 19 appropriately protected alpha-hydroxy acid equivalents of the l-alpha-amino acids, employing commercially available materials, expanding the number of available alpha-hydroxy acids from 9 to 19. PMID:14961607

  19. Parallel transport of an organic acid by solid-phase and macropore diffusion in a weakly basic ion exchanger

    SciTech Connect

    Yoshida, Hiroyuki; Takatsuji; Wataru

    2000-04-01

    The parallel transport of an organic acid by solid-phase and macropore diffusion within a porous ion exchanger was studied by measuring equilibrium isotherms and uptake curves for adsorption of acetic acid and lactic acid on a weakly basic ion exchanger, DIAION WA30. Experimental adsorption isotherms were correlated by the Langmuir equation. The Langmuir equilibrium constant of acetic acid was close to that of lactic acid, and the saturation capacity of acetic acid was about 84% that of lactic acid. Intraparticle effective diffusivity D{sub eff} was determined using the homogeneous Fickian diffusion model. The value of D{sub eff} for acetic acid was about 1.5 times lactic acid. Because D{sub eff} increased with linearly increasing bulk phase concentration C{sub 0}, D{sub eff} was separated to the solid-phase diffusivity D{sub s} and the macropore diffusivity D{sub P} by applying the parallel diffusion model. The model agreed well with the experimental curves. The values of D{sub S} and D{sub P} for acetic acid were about 2 and 1.5 times those of lactic acid, respectively. The acetic acid and the lactic acid may be separated by the difference of the diffusion rates.

  20. Selective hydrolysis of hemicellulose from wheat straw by a nanoscale solid acid catalyst.

    PubMed

    Zhong, Chao; Wang, Chunming; Huang, Fan; Wang, Fengxue; Jia, Honghua; Zhou, Hua; Wei, Ping

    2015-10-20

    A nanoscale catalyst, solid acid SO4(2-)/Fe2O3 with both Lewis and Brønsted acidity was found to effectively hydrolyze hemicellulose while keeping cellulose and lignin inactive, and selective hydrolysis of hemicellulose from wheat straw by this catalyst was also confirmed. The factors that significantly affected hydrolysis process were investigated with response surface methodology, and the optimum conditions for time, temperature, and ratio of wheat straw to catalyst (w/w) were calculated to be 4.10h, 141.97°C, and 1.95:1, respectively. A maximum hemicellulose hydrolysis yield of 63.5% from wheat straw could be obtained under these conditions. In addition, the catalyst could be recycled six times with high activity remaining. PMID:26256198

  1. Influence of propionic acid on growth and aflatoxin production by Aspergillus flavus in liquid submerged and solid substrate conditions.

    PubMed

    al-Hilli, A L; Smith, J E

    1992-01-01

    The present experiments demonstrate that sublethal concentrations of propionic acid stimulated aflatoxin production considerably in submerged shaken culture and solid substrate culture of Aspergillus flavus. In liquid conditions aflatoxin formation was significantly influenced by the time of addition of propionic acid. The spores initially swelled into large spherical cells, and the resultant hyphae developed into a swollen, stunted, and excessively branched mycelium. PMID:1573566

  2. Application of solid-acid catalyst and marine macro-algae Gracilaria verrucosa to production of fermentable sugars.

    PubMed

    Jeong, Gwi-Taek; Kim, Sung-Koo; Park, Don-Hee

    2015-04-01

    In this study, the hydrolysis of marine macro-algae Gracilaria verrucosa with a solid-acid catalyst was investigated. To optimize the hydrolysis, four reaction factors, including liquid-to-solid ratio, catalyst loading, reaction temperature, and reaction time, were investigated. In the results, the highest total reducing sugar (TRS) yield, 61 g/L (51.9%), was obtained under the following conditions: 1:7.5 solid-to-liquid ratio, 15% (w/v) catalyst loading, 140 °C reaction temperature, and 150 min reaction time. Under these conditions, 10.7 g/L of 5-HMF and 2.5 g/L of levulinic acid (LA) were generated. The application of solid-acid catalyst and marine macro-algae resources shows a very high potential for production of fermentable sugars. PMID:25625460

  3. Effects of Soluble Lignin on the Formic Acid-Catalyzed Formation of Furfural: A Case Study for the Upgrading of Hemicellulose.

    PubMed

    Dussan, Karla; Girisuta, Buana; Lopes, Marystela; Leahy, James J; Hayes, Michael H B

    2016-03-01

    A comprehensive study is presented on the conversion of hemicellulose sugars in liquors obtained from the fractionation of Miscanthus, spruce bark, sawdust, and hemp by using formic acid. Experimental tests with varying temperature (130-170 °C), formic acid concentration (10-80 wt%), carbohydrate concentrations, and lignin separation were carried out, and experimental data were compared with predictions obtained by reaction kinetics developed in a previous study. The conversions of xylose and arabinose into furfural were inherently affected by the presence of polymeric soluble lignin, decreasing the maximum furfural yields observed experimentally by up to 24%. These results were also confirmed in synthetic mixtures of pentoses with Miscanthus and commercial alkali lignin. This observation was attributed to side reactions involving intermediate stable sugar species reacting with solubilized lignin during the conversion of xylose into furfural. PMID:26805656

  4. Preparation and Absorption Spectral Property of a Multifunctional Water-Soluble Azo Compound with D-π-A Structure, 4-(4- Hydroxy-1-Naphthylazo)Benzoic Acid

    NASA Astrophysics Data System (ADS)

    Hu, L.; Lv, H.; Xie, C. G.; Chang, W. G.; Yan, Z. Q.

    2015-07-01

    A multifunctional water-soluble azo dye with the D-π-A conjugated structure, 4-(4-hydroxy-1-naphthylazo) benzoic acid ( HNBA), was designed and synthesized using 1-naphanol as the electron donator, benzoic acid as the electron acceptor, and -N=N- as the bridging group. After its structure was characterized by FTIR, 1H NMR, and element analysis, the UV-Vis absorption spectral performance of the target dye was studied in detail. The results showed that the dye, combining hydroxyl group, azo group, and carboxyl group, possessed excellent absorption spectral properties (ɛ = 1.2·104 l·mol-1·cm-1) changing with pH and solvents. In particular, in polar and protonic water, it had excellent optical response to some metal ions, i.e., Fe3+ and Pb2+, which might make it a latent colorimetric sensor for detecting heavy metal ions.

  5. Solid lipid nanoparticles as nucleic acid delivery system: properties and molecular mechanisms.

    PubMed

    de Jesus, Marcelo B; Zuhorn, Inge S

    2015-03-10

    Solid lipid nanoparticles (SLNs) have been proposed in the 1990s as appropriate drug delivery systems, and ever since they have been applied in a wide variety of cosmetic and pharmaceutical applications. In addition, SLNs are considered suitable alternatives as carriers in gene delivery. Although important advances have been made in this particular field, fundamental knowledge of the underlying mechanisms of SLN-mediated gene delivery is conspicuously lacking, an imperative requirement in efforts aimed at further improving their efficiency. Here, we address recent advances in the use of SLNs as platform for delivery of nucleic acids as therapeutic agents. In addition, we will discuss available technology for conveniently producing SLNs. In particular, we will focus on underlying molecular mechanisms by which SLNs and nucleic acids assemble into complexes and how the nucleic acid cargo may be released intracellularly. In discussing underlying mechanisms, we will, when appropriate, refer to analogous studies carried out with systems based on cationic lipids and polymers, that have proven useful in the assessment of structure-function relationships. Finally, we will give suggestions for improving SLN-based gene delivery systems, by pointing to alternative methods for SLNplex assembly, focusing on the realization of a sustained nucleic acid release. PMID:25578828

  6. Sources, solubility, and acid processing of aerosol iron and phosphorous over the South China Sea: East Asian dust and pollution outflows vs. Southeast Asian biomass burning

    NASA Astrophysics Data System (ADS)

    Hsu, S.-C.; Gong, G.-C.; Shiah, F.-K.; Hung, C.-C.; Kao, S.-J.; Zhang, R.; Chen, W.-N.; Chen, C.-C.; Chou, C. C.-K.; Lin, Y.-C.; Lin, F.-J.; Lin, S.-H.

    2014-08-01

    Iron and phosphorous are essential to marine microorganisms in vast regions in oceans worldwide. Atmospheric inputs are important allochthonous sources of Fe and P. The variability in airborne Fe deposition is hypothesized to serve an important function in previous glacial-interglacial cycles, contributing to the variability in atmospheric CO2 and ultimately the climate. Understanding the mechanisms underlying the mobilization of airborne Fe and P from insoluble to soluble forms is critical to evaluate the biogeochemical effects of these elements. In this study, we present a robust power-law correlation between fractional Fe solubility and non-sea-salt-sulfate / Total-Fe (nss-sulfate / FeT) molar ratio independent of distinct sources of airborne Fe of natural and/or anthropogenic origins over the South China Sea. This area receives Asian dust and pollution outflows and Southeast Asian biomass burning. This correlation is also valid for nitrate and total acids, demonstrating the significance of acid processing in enhancing Fe mobilization. Such correlations are also found for P, yet source dependent. These relationships serve as straightforward parameters that can be directly incorporated into available atmosphere-ocean coupling models that facilitate the assessment of Fe and P fertilization effects. Although biomass burning activity may supply Fe to the bioavailable Fe pool, pyrogenic soils are possibly the main contributors, not the burned plants. This finding warrants a multidisciplinary investigation that integrates atmospheric observations with the resulting biogeochemistry in the South China Sea, which is influenced by atmospheric forcings and nutrient dynamics with monsoons.

  7. Crystallization and preliminary X-ray analysis of the complex between a Bacillus subtilis α/β-type small acid-soluble spore protein and DNA

    SciTech Connect

    Bumbaca, Daniela; Kosman, Jeffrey; Setlow, Peter; Henderson, R. Keith; Jedrzejas, Mark J.

    2007-06-01

    An α/β-type small, acid-soluble spore protein (SASP) from Bacillus subtilis, a major source of DNA protection against damaging effects in spores, was crystallized in a functionally relevant complex with a double-stranded DNA. This report provides insights into initial characterization of the complex and its structure elucidation. An engineered variant of an α/β-type small acid-soluble spore protein (SASP) from Bacillus subtilis was crystallized in a complex with a ten-base-pair double-stranded DNA by the hanging-drop vapor-diffusion method using ammonium sulfate as a precipitating agent. Crystals grew at 281 K using sodium cacodylate buffer pH 5.5 and these crystals diffracted X-rays to beyond 2.4 Å resolution using synchrotron radiation. The crystallized complex contains two or three SASP molecules bound to one DNA molecule. The crystals belong to the hexagonal space group P6{sub 1}22 or P6{sub 5}22, with unit-cell parameters a = b = 87.0, c = 145.4 Å, α = β = 90.0, γ = 120.0°. Diffraction data were 96.6% complete to 2.4 Å resolution, with an R{sub sym} of 8.5%. Structure solution by the multiwavelength/single-wavelength anomalous dispersion method using isomorphous crystals of selenomethionine-labeled protein is in progress.

  8. Storage temperature and time influences sensory quality of mandarin oranges by altering soluble solids, acidity and aroma volatile composition

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Mandarin oranges are very prone to losing flavor quality during storage and, as a result, often have a short shelf life. To better understand the basis of this flavor loss, two mandarin varieties (‘W. Murcott’ and ‘Owari’) were stored for 0, 3 and 6 weeks at either 0 °C, 4 °C, or 8 °C plus 1 week at...

  9. Hydrolysis of Cellulose by a Mesoporous Carbon-Fe₂(SO₄)₃/γ-Fe₂O₃ Nanoparticle-Based Solid Acid Catalyst.

    PubMed

    Yamaguchi, Daizo; Watanabe, Koki; Fukumi, Shinya

    2016-01-01

    Carbon-based solid acid catalysts have shown significant potential in a wide range of applications, and they have been successfully synthesized using simple processes. Magnetically separable mesoporous carbon composites also have enormous potential, especially in separation and adsorption technology. However, existing techniques have been unable to produce a magnetically separable mesoporous solid acid catalyst because no suitable precursors have been identified. Herein we describe a magnetically separable, mesoporous solid acid catalyst synthesized from a newly developed mesoporous carbon-γ-Fe2O3 nanoparticle composite. This material exhibits an equivalent acid density and catalytic activity in the hydrolysis of microcrystalline cellulose, to that of the cellulose-derived conventional catalyst. Since it is magnetically separable, this material can be readily recovered and reused, potentially reducing the environmental impact of industrial processes to which it is applied. PMID:26856604

  10. An Investigation of Solid-State Amidization and Imidization Reactions in Vapor Deposited Poly (amic acid)

    SciTech Connect

    Anthamatten, M; Letts, S A; Day, K; Cook, R C; Gies, A P; Hamilton, T P; Nonidez, W K

    2004-06-28

    The condensation polymerization reaction of 4,4'-oxydianiline (ODA) with pyromellitic dianhydride (PMDA) to form poly(amic acid) and the subsequent imidization reaction to form polyimide were investigated for films prepared using vapor deposition polymerization techniques. Fourier-transform infrared spectroscopy (FT-IR), thermal analysis, and matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) of films at different temperatures indicate that additional solid-state polymerization occurs prior to imidization reactions. Experiments reveal that, upon vapor deposition, poly(amic acid) oligomers form that have a number-average molecular weight of about 1500 Daltons. Between 100 - 130 C these chains undergo additional condensation reaction to form slightly higher molecular weight oligomers. Calorimetry measurements show that this reaction is exothermic ({Delta}H {approx} -30 J/g) with an activation energy of about 120 kJ/mol. Experimental reaction enthalpies are compared to results from ab initio molecular modeling calculations to estimate the number of amide groups formed. At higher temperatures (150 - 300 C) imidization of amide linkages occurs as an endothermic reaction ({Delta}H {approx} +120 J/g) with an activation energy of about 130 kJ/mol. Solid-state kinetics were found to depend on reaction conversion as well as the processing conditions used to deposit films.

  11. Quantitative solid state NMR analysis of residues from acid hydrolysis of loblolly pine wood.

    PubMed

    Sievers, Carsten; Marzialetti, Teresita; Hoskins, Travis J C; Valenzuela Olarte, Mariefel B; Agrawal, Pradeep K; Jones, Christopher W

    2009-10-01

    The composition of solid residues from hydrolysis reactions of loblolly pine wood with dilute mineral acids is analyzed by (13)C Cross Polarization Magic Angle Spinning (CP MAS) NMR spectroscopy. Using this method, the carbohydrate and lignin fractions are quantified in less than 3h as compared to over a day using wet chemical methods. In addition to the quantitative information, (13)C CP MAS NMR spectroscopy provides information on the formation of additional extractives and pseudo lignin from the carbohydrates. Being a non-destructive technique, NMR spectroscopy provides unambiguous evidence of the presence of side reactions and products, which is a clear advantage over the wet chemical analytical methods. Quantitative results from NMR spectroscopy and proximate analysis are compared for the residues from hydrolysis of loblolly pine wood under 13 different conditions; samples were treated either at 150 degrees C or 200 degrees C in the presence of various acids (HCl, H(2)SO(4), H(3)PO(4), HNO(3) and TFA) or water. The lignin content determined by both methods differed on averaged by 2.9 wt% resulting in a standard deviation of 3.5 wt%. It is shown that solid degradation products are formed from saccharide precursors under harsh reaction conditions. These degradation reactions limit the total possible yield of monosaccharides from any subsequent reaction. PMID:19477123

  12. Degradation of carbohydrates during dilute sulfuric acid pretreatment can interfere with lignin measurements in solid residues.

    PubMed

    Katahira, Rui; Sluiter, Justin B; Schell, Daniel J; Davis, Mark F

    2013-04-01

    The lignin content measured after dilute sulfuric acid pretreatment of corn stover indicates more lignin than could be accounted for on the basis of the untreated corn stover lignin content. This phenomenon was investigated using a combination of (13)C cross-polarization/magic-angle spinning (CP/MAS) solid-state nuclear magnetic resonance (NMR) spectroscopy and lignin removal using acid chlorite bleaching. Only minimal contamination with carbohydrates and proteins was observed in the pretreated corn stover. Incorporating degradation products from sugars was also investigated using (13)C-labeled sugars. The results indicate that sugar degradation products are present in the pretreatment residue and may be intimately associated with the lignin. Studies comparing whole corn stover (CS) to extractives-free corn stover [CS(Ext)] clearly demonstrated that extractives are a key contributor to the high-lignin mass balance closure (MBC). Sugars and other low molecular weight compounds present in plant extractives polymerize and form solids during pretreatment, resulting in apparent Klason lignin measurements that are biased high. PMID:23428141

  13. Spray-dried solid dispersions containing ferulic acid: comparative analysis of three carriers, in vitro dissolution, antioxidant potential and in vivo anti-platelet effect.

    PubMed

    Nadal, Jessica Mendes; Gomes, Mona Lisa Simionatto; Borsato, Débora Maria; Almeida, Martinha Antunes; Barboza, Fernanda Malaquias; Zawadzki, Sônia Faria; Farago, Paulo Vitor; Zanin, Sandra Maria Warumby

    2016-11-01

    This article aimed to improve the relative solubility and dissolution rate of ferulic acid (FA) by the use of spray-dried solid dispersions (SDs) in order to ensure its in vitro antioxidant potential and to enhance its in vivo anti-platelet effect. These SDs were prepared by spray-drying at 10 and 20% of drug concentration using polyvinylpyrrolidone K30 (PVP-K30), polyethylene glycol 6000 (PEG 6000) and poloxamer-188 (PLX-188) as carriers. SDs and physical mixtures (PM) were characterized by SEM, XRPD, FTIR spectroscopy and TGA analysis. Spray-dried SDs containing FA were successfully obtained. Relative solubility of FA was improved with increasing carrier concentration. PVP-K30 and PEG 6000 formulations showed suitable drug content values close to 100%, whereas PLX-188 presented mean values between 70 and 90%. Agglomerates were observed depending on the carrier used. XRPD patterns and thermograms indicated that spray-drying led to drug amorphization and provided appropriate thermal stability, respectively. FTIR spectra demonstrated no remarkable interaction between carrier and drug for PEG 6000 and PLX-188 SDs. PVP-K30 formulations had changes in FTIR spectra, which denoted intermolecular O-H•••O = C bonds. Spray-dried SDs played an important role in enhancing dissolution rate of FA when compared to pure drug. The free radical-scavenging assay confirmed that the antioxidant activity of PEG 6000 10% SDs was kept. This formulation also provided a statistically increased in vivo anti-platelet effect compared to pure drug. In summary, these formulations enhanced relative solubility and dissolution rate of FA and chosen formulation demonstrated suitable in vitro antioxidant activity and improved in vivo anti-platelet effect. PMID:27032626

  14. Influence of solid-state acidity on the decomposition of sucrose in amorphous systems II (effect of buffer).

    PubMed

    Alkhamis, Khouloud A

    2009-04-01

    It was of interest to investigate the solid-state acidity using indicator probe molecules and sucrose degradation. Amorphous samples containing lactose, sucrose, buffers (citrate, malate, tartarate, or phosphate) with different pH values, and sodium chloride (to adjust the ionic strength) were prepared by freeze-drying. The lyophiles were characterized using powder X-ray diffraction, differential scanning calorimetry, and Karl Fischer titrimetry. The solid-state acidity of all lyophiles was measured using diffuse reflectance spectroscopy and suitable indicators (thymol blue or bromophenol blue). Selected lyophiles were subjected to a temperature of 60 degrees C and were analyzed for sucrose degradation using the Trinder kit. The results obtained from this study have shown that good correlation can be obtained between the solid-state acidity and the molar ratio of the salt and the acid in solution. The degradation of sucrose in the lyophiles is extremely sensitive to the solid-state acidity and might be able to provide a better estimate for the acidity than the indicator probe molecules. The Hammett acidity-rate profile for sucrose degradation in the lyophiles (using four different buffers) was also obtained. The profile showed similarity to the pH-rate profile in solution, and no buffer catalysis for sucrose degradation was detected in this study. PMID:19016102

  15. Molecular-Level Understanding of the Encapsulation and Dissolution of Poorly Water-Soluble Ibuprofen by Functionalized Organic Nanotubes Using Solid-State NMR Spectroscopy.

    PubMed

    Liu, Nan; Higashi, Kenjirou; Kikuchi, Junko; Ando, Shigeru; Kameta, Naohiro; Ding, Wuxiao; Masuda, Mitsutoshi; Shimizu, Toshimi; Ueda, Keisuke; Yamamoto, Keiji; Moribe, Kunikazu

    2016-05-19

    A comprehensive study of the encapsulation and dissolution of the poorly water-soluble drug ibuprofen (IBU) using two types of organic nanotubes (ONT-1 and ONT-2) was conducted. ONT-1 and ONT-2 had similar inner and outer diameters, but these surfaces were functionalized with different groups. IBU was encapsulated by each ONT via solvent evaporation. The amount of IBU in the ONTs was 9.1 and 29.2 wt % for ONT-1 and ONT-2, respectively. Dissolution of IBU from ONT-1 was very rapid, while from ONT-2 it was slower after the initial burst release. One-dimensional (1D) (1)H, (13)C, and two-dimensional (2D) (1)H-(13)C solid-state NMR measurements using fast magic-angle spinning (MAS) at a rate of 40 kHz revealed the molecular state of the encapsulated IBU in each ONT. Extremely mobile IBU was observed inside the hollow nanosapce of both ONT-1 and ONT-2 using (13)C MAS NMR with a single pulse (SP) method. Interestingly, (13)C cross-polarization (CP) MAS NMR demonstrated that IBU also existed on the outer surface of both ONTs. The encapsulation ratios of IBU inside the hollow nanospaces versus on the outer surfaces were calculated by waveform separation to be approximately 1:1 for ONT-1 and 2:1 for ONT-2. Changes in (13)C chemical shifts showed the intermolecular interactions between the carboxyl group of IBU and the amino group on the ONT-2 inner surface. The cationic ONT-2 could form the stronger electrostatic interactions with IBU in the hollow nanosapce than anionic ONT-1. On the other hand, 2D (1)H-(13)C NMR indicated that the hydroxyl groups of the glucose unit on the outer surface of the ONTs interacted with the carboxyl group of IBU in both ONT-1 and ONT-2. The changes in peak shape and chemical shift of the ONT glucose group after IBU encapsulation were larger in ONT-2 than in ONT-1, indicating a stronger interaction between IBU and the outer surface of ONT-2. The smaller amount of IBU encapsulation and rapid IBU dissolution from ONT-1 could be due to the weak

  16. Diurnal and temporal variations of water-soluble dicarboxylic acids and related compounds in aerosols from the northern vicinity of Beijing: implication for photochemical aging during atmospheric transport.

    PubMed

    He, Nannan; Kawamura, Kimitaka; Okuzawa, K; Pochanart, P; Liu, Y; Kanaya, Y; Wang, Z F

    2014-11-15

    Aerosol samples were collected in autumn 2007 on day- and nighttime basis in the northern receptor site of Beijing, China. The samples were analyzed for total carbon (TC) and water-soluble dicarboxylic acids (C2-C12), oxocarboxylic acids (C2-C9), glyoxal and methylglyoxal to better understand the photochemical aging of organic aerosols in the vicinity of Beijing. Concentrations of TC are 50% greater in daytime when winds come from Beijing than in nighttime when winds come from the northern forest areas. Most diacids showed higher concentrations in daytime, suggesting that the organics emitted from the urban Beijing and delivered to the northern vicinity in daytime are subjected to photo-oxidation to result in diacids. However, oxalic acid (C2), which is the most abundant diacid followed by C3 or C4, became on average 30% more abundant in nighttime together with azelaic, ω-oxooctanoic and ω-oxononanoic acids, which are specific oxidation products of biogenic unsaturated fatty acids. Methylglyoxal, an oxidation product of isoprene and a precursor of oxalic acid, also became 29% more abundant in nighttime. Based on a positive correlation between C2 and glyoxylic acid (ωC2) in nighttime when relative humidity significantly enhanced, we propose a nighttime aqueous phase production of C2 via the oxidation of ωC2. We found an increase in the contribution of diacids to TC by 3 folds during consecutive clear days. This study demonstrates that diacids and related compounds are largely produced in the northern vicinity of Beijing via photochemical processing of organic precursors emitted from urban center and forest areas. PMID:25181047

  17. Kinetics of liquid-solid reactions in naphthenic acid conversion and Kraft pulping

    NASA Astrophysics Data System (ADS)

    Yang, Ling

    Two liquid-solid reactions, in which the morphology of the solid changes as the reactions proceeds, were examined. One is the NA conversion in oil by decarboxylation on metal oxides and carbonates, and the other is the Kraft pulping in which lignin removal by delignification reaction. In the study of the NA conversion, CaO was chosen as the catalyst for the kinetic study from the tested catalysts based on NA conversion. Two reaction mixtures, carrier oil plus commercial naphthenic acids and heavy vacuum gas oil (HVGO) from Athabasca bitumen, were applied in the kinetic study. The influence of TAN, temperature, and catalyst loading on the NA conversion and decarboxylation were studied systematically. The results showed that the removal rate of TAN and the decarboxylation of NA were both independent of the concentration of NA over the range studied, and significantly dependent on reaction temperature. The data from analyzing the spent catalyst demonstrated that calcium naphthenate was an intermediate of the decarboxylation reaction of NA, and the decomposition of calcium naphthenate was a rate-determining step. In the study on the delignification of the Kraft pulping, a new mechanism was proposed for the heterogeneous delignification reaction during the Kraft pulping process. In particular, the chemical reaction mechanism took into account the heterogeneous nature of Kraft pulping. Lignin reacted in parallel with sodium hydroxide and sodium sulfide. The mechanism consists of three key kinetic steps: (1) adsorption of hydroxide and hydrosulfide ions on lignin; (2) surface reaction on the solid surface to produce degraded lignin products; and (3) desorption of degradation products from the solid surface. The most important step for the delignification process is the surface reaction, rather than the reactions occurring in the liquid phase. A kinetic model has, thus, been developed based on the proposed mechanism. The derived kinetic model showed that the mechanism

  18. Potential effects of clean coal technologies on acid precipitation, greenhouse gases, and solid waste disposal

    SciTech Connect

    Blasing, T.J.; Miller, R.L.; McCold, L.N.

    1993-11-01

    The US Department of Energy`s (DOE`s) Clean Coal Technology Demonstration Program (CCTDP) was initially funded by Congress to demonstrate more efficient, economically feasible, and environmentally acceptable coal technologies. Although the environmental focus at first was on sulfur dioxide (SO{sub 2}) and nitrogen oxides (NO{sub x}) because their relationship to acid precipitation, the CCTDP may also lead to reductions in carbon dioxide (CO{sub 2}) emissions and in the volume of solid waste produced, compared with conventional technologies. The environmental effects of clean coal technologies (CCTs) depend upon which (if any) specific technologies eventually achieve high acceptance in the marketplace. In general, the repowering technologies and a small group of retrofit technologies show the most promise for reducing C0{sub 2} emissions and solid waste. These technologies also compare favorably with other CCTs in terms of SO{sub 2} and NO{sub x} reductions. The upper bound for CO{sup 2} reductions in the year 2010 is only enough to reduce global ``greenhouse`` warming potential by about 1%. However, CO{sub 2} emissions come from such variety of sources around the globe that no single technological innovation or national policy change could realistically be expected to reduce these emissions by more than a few percent. Particular CCTs can lead to either increases or decreases in the amount of solid waste produced. However, even if decreases are not achieved, much of the solid waste from clean coal technologies would be dry and therefore easier to dispose of than scrubber sludge.

  19. PuPO4(cr, hyd.) Solubility Product and Pu3+ Complexes With Phosphate and Ethylenediaminetetraacetic Acid

    SciTech Connect

    Rai, Dhanpat; Moore, Dean A.; Felmy, Andrew R.; Rosso, Kevin M.; Bolton, Harvey

    2010-06-15

    To determine the solubility product of PuPO4(cr, hyd.) and the complexation constants of Pu(III) with phosphate and EDTA, the solubility of PuPO4(cr, hyd.) was investigated as a function of: 1) time and pH varying from 1.0 to 12.0 and at a fixed 0.00032 M phosphate concentration; 2) NaH2PO4 concentrations varying from 0.0001 M to 1.0 M and at a fixed pH value of 2.5; 3) time and pH varying from 1.3 to 13.0 at fixed concentrations of 0.00032 M phosphate and 0.0004 M or 0.002 M Na2H2EDTA; and 4) Na2H2EDTA concentrations varying from 0.00005 M to 0.0256 M at a fixed 0.00032 M phosphate concentration and at pH values of approximately 3.5, 10.6, and 12.6. A combination of solvent extraction and spectrophotometric techniques confirmed that the use of hydroquinone and Na2S2O4 helped maintain Pu as Pu(III). The solubility data were interpreted using Pitzer and SIT models, and both provided similar values for the solubility product of PuPO4(cr, hyd.) and for the formation constant of PuEDTA-. The log10 of the solubility product of PuPO4(cr, hyd.) (PuPO4(cr, hyd.) = Pu3+ + PO4 ) was determined to be –(24.42 ± 0.38). Pitzer modeling showed that phosphate interactions with Pu3+ were extremely weak and did not require any phosphate complexes (e.g., PuPO4(aq), PuH2PO42+, Pu(H2PO4)2+, Pu(H2PO4)3(aq), and Pu(H2PO4)4-), as proposed in existing literature, to explain the experimental data. SIT modeling, however, required the inclusion of PuH2PO42+ to explain the data in high NaH2PO4 concentrations; this illustrates the differences one can expect when using these two chemical models to interpret the data. As the Pu(III)-EDTA species, only PuEDTA- was needed to interpret the experimental data in a large range in pH values (1.3–12.9) and EDTA concentrations (0.00005–0.256 M). Calculations based on density functional theory support the existence of PuEDTA- (with prospective stoichiometry as Pu(OH2)3EDTA-) as the chemically and structurally stable species. The log10 of the

  20. Characterizing the acid/base behavior of oil-soluble surfactants at the interface of nonpolar solvents with a polar phase.

    PubMed

    Lee, Joohyung; Zhou, Zhang-Lin; Behrens, Sven Holger

    2015-06-01

    We propose a simple method of characterizing the (Lewis) acid/base behavior of oil-soluble nonionic surfactants at the interface of nonpolar solvents with a polar phase. Using interfacial tensiometry, we probe the effective acidic and basic response of nonpolar surfactant solutions to contact with a variety of polar reference liquids. The measured interfacial tensions are used as experimental coefficients in a set of equations borrowed from the thermodynamic "surface energy component model" of van Oss, Chaudhury, and Good (vOCG), but used here in a more heuristic fashion and with a revised interpretation of the parameters extracted to describe the dispersive, acidic, and basic character of the sample. We test the proposed characterization method using alkane solutions of purified polyisobutylene succinimide (PIBS) surfactants with systematic structural variations, and observe that the inferred parameter values are consistent with, and sensitive to, subtle differences in the surfactant chemistry. This suggests the possibility to compare different surfactant solutions semiquantitatively with regard to their acidic and basic character. In a further illustration of the proposed analysis, we characterize a solution of commercial PIBS surfactant in hexane, and find that the parameters obtained by the proposed method correctly predict the solution interfacial tension with a polar liquid not included among the chosen reference liquids. PMID:25978798

  1. Enhanced anti-cancer efficacy to cancer cells by doxorubicin loaded water-soluble amino acid-modified β-cyclodextrin platinum complexes.

    PubMed

    Zhao, Mei-Xia; Zhao, Meng; Zeng, Er-Zao; Li, Yang; Li, Jin-Ming; Cao, Qian; Tan, Cai-Ping; Ji, Liang-Nian; Mao, Zong-Wan

    2014-08-01

    The effective targeted delivery of insoluble anticancer drugs to increase the intracellular drug concentration has become a focus in cancer therapy. In this system, two water-soluble amino acid-modified β-cyclodextrin (β-CD) platinum complexes were reported. They showed preferable binding ability to DNA and effective inhibition to cancer cells, and they could bind and unwind pBR322 DNA in a manner which was similar to cisplatin. Besides, our platinum complexes could effectively deliver the anticancer drug doxorubicin (Dox) into cells and had higher cell inhibition ratio, but less toxicity on the normal cells, compared with cancer cells. In this combination system, Dox was encapsulated into the hydrophobic cavities of β-CD at the optimum molar ratio of 1:1, which were validated by UV-visible (UV-vis) absorption spectroscopy, fluorescence spectroscopy and MTT experiments. Moreover, the combination system had higher cell inhibition ratio than free Dox and amino acid-modified β-CD platinum complexes, and the results of high content screening (HCS) showed that Dox-loaded amino acid-modified β-CD platinum complexes could permeate the cell membrane and enter cells, suggesting the efficient transport of Dox across the membranes with the aid of the β-CD. We expect that the amino acid-modified β-CD platinum complexes will deliver the antitumor drug Dox to enhance intracellular drug accumulation and such combination system showed great potential as an antitumor drug. PMID:24803024

  2. Sense-, antisense- and RNAi-4CL1 regulate soluble phenolic acids, cell wall components and growth in transgenic Populus tomentosa Carr.

    PubMed

    Tian, Xiaoming; Xie, Jin; Zhao, Yanling; Lu, Hai; Liu, Shichang; Qu, Long; Li, Jianmei; Gai, Ying; Jiang, Xiangning

    2013-04-01

    Regulation of lignin biosynthesis affects plant growth and wood properties. Transgenic downregulation of 4-coumarate:coenzyme A ligase (4CL, EC 6.2.1.12) may reduce lignin content in cell walls, which could improve the qualities of pulp in papermaking and increase the efficiency of bioenergy applications. To determine the effects of Ptc4CL1 on lignin biosynthesis and plant growth, Populus tomentosa Carr. was transformed using sense-, antisense-, and RNAi-4CL1 genes. The growth properties, gene expression, enzyme activity, lignin content and composition and content of soluble phenolic acids were investigated in 1-year-old field-grown transgenic poplar trees. Transgenic up- and down-regulation of 4CL1 altered lignin content and composition in transgenic poplars, but there were no negative effects on the growth of transgenic plants. In addition, the severe changes in auxin observed in transgenic lines led to significantly enhanced growth performance. Furthermore, lignin content was tightly correlated with the alteration of 4CL1 enzymatic activity, which was correlated with 4CL1 gene expression. A significant increase in S units in lignin with a slight increase in sinapic acid was observed in 4CL1 down-regulated transgenic poplars. These results suggest that 4CL1 is a traffic control gene in monolignol biosynthesis and confirm that 4CL1 activity has been implicated with sinapoyl activation. Finally, our data demonstrate that there is cross-correlation among 4CL1 gene expression, 4CL1 enzyme activity, soluble phenolic acid, lignin monomer biosynthesis, and lignin content. PMID:23434928

  3. On the gas-particle partitioning of soluble organic aerosol in two urban atmospheres with contrasting emissions: 2. Gas and particle phase formic acid

    NASA Astrophysics Data System (ADS)

    Liu, Jiumeng; Zhang, Xiaolu; Parker, Eric T.; Veres, Patrick R.; Roberts, James M.; de Gouw, Joost A.; Hayes, Patrick L.; Jimenez, Jose L.; Murphy, Jennifer G.; Ellis, Raluca A.; Huey, L. Greg; Weber, Rodney J.

    2012-10-01

    Gas and fine particle (PM2.5) phase formic acid concentrations were measured with online instrumentation during separate one-month studies in the summer of 2010 in Los Angeles (LA), CA, and Atlanta, GA. In both urban environments, median gas phase concentrations were on the order of a few ppbv (LA 1.6 ppbv, Atlanta 2.3 ppbv) and median particle phase concentrations were approximately tens of ng/m3 (LA 49 ng/m3, Atlanta 39 ng/m3). LA formic acid gas and particle concentrations had consistent temporal patterns; both peaked in the early afternoon and generally followed the trends in photochemical secondary gases. Atlanta diurnal trends were more irregular, but the mean diurnal profile had similar afternoon peaks in both gas and particle concentrations, suggesting a photochemical source in both cities. LA formic acid particle/gas (p/g) ratios ranged between 0.01 and 12%, with a median of 1.3%. No clear evidence that LA formic acid preferentially partitioned to particle water was observed, except on three overcast periods of suppressed photochemical activity. Application of Henry's Law to predict partitioning during these periods greatly under-predicted particle phase formate concentrations based on bulk aerosol liquid water content (LWC) and pH estimated from thermodynamic models. In contrast to LA, formic acid partitioning in Atlanta appeared to be more consistently associated with elevated relative humidity (i.e., aerosol LWC), although p/g ratios were somewhat lower, ranging from 0.20 to 5.8%, with a median of 0.8%. Differences in formic acid gas absorbing phase preferences between these two cities are consistent with that of bulk water-soluble organic carbon reported in a companion paper.

  4. On the gas-particle partitioning of soluble organic aerosol in two urban atmospheres with contrasting emissions: 2. Gas and particle phase formic acid

    NASA Astrophysics Data System (ADS)

    Liu, Jiumeng; Zhang, Xiaolu; Parker, Eric T.; Veres, Patrick R.; Roberts, James M.; Gouw, Joost A.; Hayes, Patrick L.; Jimenez, Jose L.; Murphy, Jennifer G.; Ellis, Raluca A.; Huey, L. Greg; Weber, Rodney J.

    2011-11-01

    Gas and fine particle (PM2.5) phase formic acid concentrations were measured with online instrumentation during separate one-month studies in the summer of 2010 in Los Angeles (LA), CA, and Atlanta, GA. In both urban environments, median gas phase concentrations were on the order of a few ppbv (LA 1.6 ppbv, Atlanta 2.3 ppbv) and median particle phase concentrations were approximately tens of ng/m3 (LA 49 ng/m3, Atlanta 39 ng/m3). LA formic acid gas and particle concentrations had consistent temporal patterns; both peaked in the early afternoon and generally followed the trends in photochemical secondary gases. Atlanta diurnal trends were more irregular, but the mean diurnal profile had similar afternoon peaks in both gas and particle concentrations, suggesting a photochemical source in both cities. LA formic acid particle/gas (p/g) ratios ranged between 0.01 and 12%, with a median of 1.3%. No clear evidence that LA formic acid preferentially partitioned to particle water was observed, except on three overcast periods of suppressed photochemical activity. Application of Henry's Law to predict partitioning during these periods greatly under-predicted particle phase formate concentrations based on bulk aerosol liquid water content (LWC) and pH estimated from thermodynamic models. In contrast to LA, formic acid partitioning in Atlanta appeared to be more consistently associated with elevated relative humidity (i.e., aerosol LWC), although p/g ratios were somewhat lower, ranging from 0.20 to 5.8%, with a median of 0.8%. Differences in formic acid gas absorbing phase preferences between these two cities are consistent with that of bulk water-soluble organic carbon reported in a companion paper.

  5. Improved In Vitro Antileukemic Activity of All-Trans Retinoic Acid Loaded in Cholesteryl Butyrate Solid Lipid Nanoparticles.

    PubMed

    Silva, Elton Luiz; Lima, Flávia Alves; Carneiro, Guilherme; Ramos Jonas Periera; Gomes, Dawidson Assis; de Souza-Fagundes, Elaine Maria; Ferreira, Lucas Antônio Miranda

    2016-02-01

    All-trans retinoic acid, a hydrophobic drug, has become one of the most successful examples of differentiation agents used for treatment of acute promyelocytic leukemia. On the other hand, histone deacetylase inhibitors, such as cholesteryl butyrate, present differentiating activity and.can potentiate action of drugs such as all-trans retinoic acid. Solid lipid nanoparticles represent a promising alternative for administration of hydrophobic drugs such as ATRA. This study aimed to develop, characterize, and evaluate the cytotoxicity of all-trans retinoic acid-loaded solid lipid nanoparticles for leukemia treatment. The influence of in situ formation of an ion pairing between all-trans retinoic acid and lipophilic amines on the characteristics of the particles (size, zeta potential, encapsulation efficiency) was evaluated. Cholesteryl butyrate, a butyric acid donor, was used as a component of the lipid matrix. In vitro activity on cell viability and distribution of cell cycle phases were evaluated for HL-60, Jurkat, and THP-1 cell lines. The encapsulation efficiency of all-trans retinoic acid in cholesteryl butyrate-solid lipid nanoparticles was significantly increased by the presence of the amine. Inhibition of cell viability by all-trans retinoic acid-loaded solid lipid nanoparticles was more pronounced than the free drug. Analysis of the distribution of cell cycle phases also showed increased activity for all-trans retinoic acid-loaded cholesteryl butyrate-solid lipid nanoparticles, with a clear increase in subdiploid DNA content. The ion pair formation in SLN containing cholesteryl butyrate can be explored as a simple and inexpensive strategy to improve the efficacy and bioavail-ability of ATRA in the treatment of the cancer and metabolic diseases in which this retinoid plays an important role. PMID:27433579

  6. Accelerated healing of cutaneous leishmaniasis in non-healing BALB/c mice using water soluble amphotericin B-polymethacrylic acid

    PubMed Central

    Corware, Karina; Harris, Debra; Teo, Ian; Rogers, Matthew; Naresh, Kikkeri; Müller, Ingrid; Shaunak, Sunil

    2011-01-01

    Cutaneous leishmaniasis (CL) is a neglected tropical disease that causes prominent skin scaring. No water soluble, non-toxic, short course and low cost treatment exists. We developed a new water soluble amphotericin B-polymethacrylic acid (AmB-PMA) using established and scalable chemistries. AmB-PMA was stable for 9 months during storage. In vitro, it was effective against Leishmania spp. promastigotes and amastigote infected macrophages. It was also less toxic and more effective than deoxycholate-AmB, and similar to liposomal AmB. Its in vivo activity was determined in both early and established CL lesion models of Leishmania major infection in genetically susceptible non-healing BALB/c mice. Intradermal AmB-PMA at a total dose of 18 mg of AmB/kg body weight led to rapid parasite killing and lesion healing. No toxicity was seen. No parasite relapse occurred after 80 days follow-up. Histological studies confirmed rapid parasite clearance from macrophages followed by accelerated fibroblast mediated tissue repair, regeneration and cure of the infection. Quantitative mRNA studies of the CL lesions showed that accelerated healing was associated with increased Tumor Necrosis Factor-α and Interferon-γ, and reduced Interleukin-10. These results suggest that a cost-effective AmB-PMA could be used to pharmacologically treat and immunotherapeutically accelerate the healing of CL lesions. PMID:21807409

  7. Microwave Effect for Glycosylation Promoted by Solid Super Acid in Supercritical Carbon Dioxide

    PubMed Central

    Hinou, Hiroshi; Saito, Naohiro; Ogawa, Masato; Maeda, Takahiko; Nishimura, Shin-Ichiro

    2009-01-01

    The effects of microwave irradiation (2.45 GHz, 200 W) on glycosylation promoted by a solid super acid in supercritical carbon dioxide was investigated with particular attention paid to the structure of the acceptor substrate. Because of the symmetrical structure and high diffusive property of supercritical carbon dioxide, microwave irradiation did not alter the temperature of the reaction solution, but enhanced reaction yield when aliphatic acceptors are employed. Interestingly, the use of a phenolic acceptor under the same reaction conditions did not show these promoting effects due to microwave irradiation. In the case of aliphatic diol acceptors, the yield seemed to be dependent on the symmetrical properties of the acceptors. The results suggest that microwave irradiation do not affect the reactivity of the donor nor promoter independently. We conclude that the effect of acceptor structure on glycosylation yield is due to electric delocalization of hydroxyl group and dielectrically symmetric structure of whole molecule. PMID:20054471

  8. Mesoporous nickel-aluminosilicate nanocomposite: a solid acid catalyst for ether synthesis.

    PubMed

    Neelakandeswari, N; Karvembu, R; Dharmaraj, N

    2013-04-01

    Mesoporous nickel aluminosilicate, a solid acid catalyst prepared by sol-gel technique was utilized as a heterogeneous catalyst for the synthesis of symmetrical ethers by dehydro-condensation of alcohols. The prepared catalysts were characterized by Fourier-transform infra red spectroscopy (FT-IR), powder X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDAX), N2 adsorption-desorption analysis, temperature programmed desorption of ammonia (TPD) and X-ray photoelectron spectroscopic techniques. The presence of the catalyst assisted the etherification reaction in 30 minutes. Ethers formed in these reactions were quantified by gas chromatography (GC) and the identities of few of them were confirmed by nuclear magnetic resonance spectral data (NMR). PMID:23763171

  9. NEXAFS Chemical State and Bond Lengths of p-Aminobenzoic Acid in Solution and Solid State

    NASA Astrophysics Data System (ADS)

    Stevens, J. S.; Gainar, A.; Suljoti, E.; Xiao, J.; Golnak, R.; Aziz, E. F.; Schroeder, S. L. M.

    2016-05-01

    Solid-state and solution pH-dependent NEXAFS studies allow direct observation of the electronic state of para-aminobenzoic acid (PABA) as a function of its chemical environment, revealing the chemical state and bonding of the chemical species. Variations in the ionization potential (IP) and 1s→π* resonances unequivocally identify the chemical species (neutral, cationic, or anionic) present and the varying local environment. Shifts in σ* shape resonances relative to the IP in the NEXAFS spectra vary with C-N bond length, and the important effect of minor alterations in bond length is confirmed with nitrogen FEFF calculations, leading to the possibility of bond length determination in solution.

  10. Novel solid state proton-conductors based on polymeric non-oxy acids. Final report

    SciTech Connect

    Appleby, A.J.; Srinivasan, S.; Parthasarathy, A.; Gonzalez, E.R.; DesMarteau, D.; Gillette, M.S.; Ghosh, J.K.; Jalan, V.; Desai, M.

    1992-01-01

    Objectives of this project were to prepare and characterize novel solid state proton-conductors and to evaluate these compounds as fuel cell electrolytes. The thrust was on the synthesis of new proton-conducting ``model`` and ``polymeric`` compounds, based on acid functions of the type (R{sub f}SO{sub 2}){sub 2}NH and (R{sub f}SO{sub 2}){sub 2}CH{sub 2} in appropriate fluorinated carbon structures, their physics-chemical characterization (Infra-red, Nuclear Magnetic Resonance, Differential Scanning Calorimetry, and X-ray Diffraction), and is pro. evaluation as candidate fuel cell electrolytes for use at elevated temperatures. This project consisted of four tasks (i) Synthesis of Proton-Conducting Polymer Electrolytes; (ii) Physical and Chemical Characterization of Proton-Conducting Polymer Electrolytes; (iii) Electrochemical Characterization of Proton-Conducting Polymer Electrolytes; and (iv) Evaluation of Proton-Conducting Polymer Electrolytes for Fuel Cells.

  11. Experimental and computational thermochemical study and solid-phase structure of 5,5-dimethylbarbituric acid.

    PubMed

    Roux, María Victoria; Notario, Rafael; Foces-Foces, Concepción; Temprado, Manuel; Ros, Francisco; Emel'yanenko, Vladimir N; Verevkin, Sergey P

    2010-03-18

    This paper reports an experimental and computational thermochemical study on 5,5-dimethylbarbituric acid and the solid-phase structure of the compound. The value of the standard (p(o) = 0.1 MPa) molar enthalpy of formation in the gas phase at T = 298.15 K has been determined. The energy of combustion was measured by static bomb combustion calorimetry, and from the result obtained, the standard molar enthalpy of formation in the crystalline state at T = 298.15 K was calculated as -(706.4 +/- 2.2) kJ x mol(-1). The enthalpy of sublimation was determined using a transference (transpiration) method in a saturated NB(2) stream, and a value of the enthalpy of sublimation at T = 298.15 K was derived as (115.8 +/- 0.5) kJ x mol(-1). From these results a value of -(590.6 +/- 2.3) kJ x mol(-1) for the gas-phase enthalpy of formation at T = 298.15 K was determined. Theoretical calculations at the G3 level were performed, and a study on molecular and electronic structure of the compound has been carried out. Calculated enthalpies of formation are in reasonable agreement with the experimental value. 5,5-Dimethylbarbituric acid was characterized by single crystal X-ray diffraction analysis. In the crystal structure, N-H...O=C hydrogen bonds lead to the formation of ribbons connected further by weak C-H...O=C hydrogen bonds into a three-dimensional network. The molecular and supramolecular structures observed in the solid state were also investigated in the gas phase by DFT calculations. PMID:20180529

  12. Characterization and dynamic properties for the solid inclusion complexes of β-cyclodextrin and perfluorooctanoic acid.

    PubMed

    Karoyo, Abdalla H; Sidhu, Paul; Wilson, Lee D; Hazendonk, Paul

    2013-07-11

    The structural characterization and dynamic properties of solid-state inclusion complexes (ICs) formed between β-cyclodextrin (β-CD; host) and perfluorooctanoic acid (PFOA; guest) were investigated using (13)C NMR spectroscopy. The 1:1 and 2:1 host/guest solid-state complexes were prepared using a modified dissolution method to obtain complexes with high phase purity. These complexes were further characterized using differential scanning calorimetry (DSC), FT-IR spectroscopy, powder X-ray diffraction (PXRD), (19)F directpolarization (DP), and (13)C cross-polarization (CP) with magic-angle spinning (MAS) NMR spectroscopy. The (19)F → (13)C CP results provided unequivocal support for the formation of well-defined inclusion compounds. The phase purity of the complexes formed between β-CD and PFOA were assessed using the (19)F DP NMR technique at variable temperature (VT) and MAS at 20 kHz. The complexes were found to be of high phase purity when prepared in accordance with the modified dissolution method. The motional dynamics of the guest in the solid complexes were assessed using T1/T2/T1ρ relaxation NMR methods at ambient and VT conditions. The relaxation data revealed reliable and variable guest dynamics for the 1:1 versus 2:1 complexes at the VTs investigated. The motional dynamics of the guest molecules involve an ensemble of axial motions of the whole chain and 120° rotational jumps of the methyl (CF3) group at the termini of the perfluorocarbon chain. The axial and rotational dynamics of the guest in the 1:1 and 2:1 complexes differ in distribution and magnitude in accordance with the binding geometry of the guest within the host. PMID:23713518

  13. Reducing acid leaching of manganiferous ore: effect of the iron removal operation on solid waste disposal.

    PubMed

    De Michelis, Ida; Ferella, Francesco; Beolchini, Francesca; Vegliò, Francesco

    2009-01-01

    The process of reducing acid leaching of manganiferous ore is aimed at the extraction of manganese from low grade manganese ores. This work is focused on the iron removal operation. The following items have been considered in order to investigate the effect of the main operating conditions on solid waste disposal and on the process costs: (i) type and quantity of the base agent used for iron precipitation, (ii) effective need of leaching waste separation prior to the iron removal operation, (iii) presence of a second leaching stage with the roasted ore, which might also act as a preliminary iron removal step, and (iv) effect of tailings washing on the solid waste classification. Different base compounds have been tested, including CaO, CaCO3, NaOH, and Na2CO3. The latter gave the best results concerning both the precipitation process kinetics and the reagent consumption. The filtration of the liquor leach prior to iron removal was not necessary, implying significant savings in capital costs. A reduction of chemical consumption and an increase of manganese concentration in the solution were obtained by introducing secondary leaching tests with the previously roasted ore; this additional step was introduced without a significant decrease of global manganese extraction yield. Finally, toxicity characteristic leaching procedure (TCLP) tests carried out on the leaching solid waste showed: (i) a reduction of arsenic mobility in the presence of iron precipitates, and (ii) the need for a washing step in order to produce a waste that is classifiable as not dangerous, taking into consideration the existing Environmental National Laws. PMID:18556190

  14. Reducing acid leaching of manganiferous ore: Effect of the iron removal operation on solid waste disposal

    SciTech Connect

    De Michelis, Ida; Ferella, Francesco; Beolchini, Francesca Veglio, Francesco

    2009-01-15

    The process of reducing acid leaching of manganiferous ore is aimed at the extraction of manganese from low grade manganese ores. This work is focused on the iron removal operation. The following items have been considered in order to investigate the effect of the main operating conditions on solid waste disposal and on the process costs: (i) type and quantity of the base agent used for iron precipitation, (ii) effective need of leaching waste separation prior to the iron removal operation, (iii) presence of a second leaching stage with the roasted ore, which might also act as a preliminary iron removal step, and (iv) effect of tailings washing on the solid waste classification. Different base compounds have been tested, including CaO, CaCO{sub 3}, NaOH, and Na{sub 2}CO{sub 3}. The latter gave the best results concerning both the precipitation process kinetics and the reagent consumption. The filtration of the liquor leach prior to iron removal was not necessary, implying significant savings in capital costs. A reduction of chemical consumption and an increase of manganese concentration in the solution were obtained by introducing secondary leaching tests with the previously roasted ore; this additional step was introduced without a significant decrease of global manganese extraction yield. Finally, toxicity characteristic leaching procedure (TCLP) tests carried out on the leaching solid waste showed: (i) a reduction of arsenic mobility in the presence of iron precipitates, and (ii) the need for a washing step in order to produce a waste that is classifiable as not dangerous, taking into consideration the existing Environmental National Laws.

  15. Removing hydrochloric acid exhaust products from high performance solid rocket propellant using aluminum-lithium alloy.

    PubMed

    Terry, Brandon C; Sippel, Travis R; Pfeil, Mark A; Gunduz, I Emre; Son, Steven F

    2016-11-01

    Hydrochloric acid (HCl) pollution from perchlorate based propellants is well known for both launch site contamination, as well as the possible ozone layer depletion effects. Past efforts in developing environmentally cleaner solid propellants by scavenging the chlorine ion have focused on replacing a portion of the chorine-containing oxidant (i.e., ammonium perchlorate) with an alkali metal nitrate. The alkali metal (e.g., Li or Na) in the nitrate reacts with the chlorine ion to form an alkali metal chloride (i.e., a salt instead of HCl). While this technique can potentially reduce HCl formation, it also results in reduced ideal specific impulse (ISP). Here, we show using thermochemical calculations that using aluminum-lithium (Al-Li) alloy can reduce HCl formation by more than 95% (with lithium contents ≥15 mass%) and increase the ideal ISP by ∼7s compared to neat aluminum (using 80/20 mass% Al-Li alloy). Two solid propellants were formulated using 80/20 Al-Li alloy or neat aluminum as fuel additives. The halide scavenging effect of Al-Li propellants was verified using wet bomb combustion experiments (75.5±4.8% reduction in pH, ∝ [HCl], when compared to neat aluminum). Additionally, no measurable HCl evolution was detected using differential scanning calorimetry coupled with thermogravimetric analysis, mass spectrometry, and Fourier transform infrared absorption. PMID:27289269

  16. Treatment of acid mine drainage with anaerobic solid-substrate reactors

    SciTech Connect

    Drury, W.J.

    1999-10-01

    Anaerobic solid-substrate reactors were used in a laboratory study of acid mine drainage treatment. Parallel systems were run continuously for 23 months, both containing a solid substrate of 2:1 (weight) cow manure and sawdust. One system had cheese whey added with the mine drainage to provide an additional electron donor source to simulate sulfate-reducing bacteria activity. Effluent pH from the reactor with whey addition was relatively constant at 6.5. Effluent pH from the reactor without whey addition dropped over time from 6.7 to approximately 5.5. Whey addition increased effluent alkalinity [550 to 700 mg/L as calcium carbonate (CaCO{sub 3}) versus 50 to 300 mg/L as CaCO{sub 3}] and sulfate removal (98 to 80% versus 60 to 40%). Sulfate removal rate with whey addition decreased over time from 250 to 120 mmol/m{sup 3}{center{underscore}dot}d, whereas it decreased from 250 to 40 mmol/m{sup 3}{center{underscore}dot}d without whey addition. Whey addition increased removal of dissolved iron, dissolved manganese, and dissolved zinc in the second part of the experiment. Copper and cadmium removals were greater than 99%, and arsenic removal was 84% without whey addition and 89% with whey addition. Effluent sulfide concentrations were approximately 1 order of magnitude greater with whey addition. A 63-day period of excessive loading permanently decreased treatment efficiency without whey addition.

  17. Characterization and Determination of Origin of Lactic Acid Bacteria from a Sorghum-Based Fermented Weaning Food by Analysis of Soluble Proteins and Amplified Fragment Length Polymorphism Fingerprinting

    PubMed Central

    Kunene, Nokuthula F.; Geornaras, Ifigenia; von Holy, Alexander; Hastings, John W.

    2000-01-01

    The group that includes the lactic acid bacteria is one of the most diverse groups of bacteria known, and these organisms have been characterized extensively by using different techniques. In this study, 180 lactic acid bacterial strains isolated from sorghum powder (44 strains) and from corresponding fermented (93 strains) and cooked fermented (43 strains) porridge samples that were prepared in 15 households were characterized by using biochemical and physiological methods, as well as by analyzing the electrophoretic profiles of total soluble proteins. A total of 58 of the 180 strains were Lactobacillus plantarum strains, 47 were Leuconostoc mesenteroides strains, 25 were Lactobacillus sake-Lactobacillus curvatus strains, 17 were Pediococcus pentosaceus strains, 13 were Pediococcus acidilactici strains, and 7 were Lactococcus lactis strains. L. plantarum and L. mesenteroides strains were the dominant strains during the fermentation process and were recovered from 87 and 73% of the households, respectively. The potential origins of these groups of lactic acid bacteria were assessed by amplified fragment length polymorphism fingerprint analysis. PMID:10698775