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Sample records for monohydrate c9h9n2cu4cl7oc9h8n23xh2o hexa-mu2-chloro-mu4-oxo-tetrakispyridine

  1. 21 CFR 168.111 - Dextrose monohydrate.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 2 2010-04-01 2010-04-01 false Dextrose monohydrate. 168.111 Section 168.111 Food... Table Sirups § 168.111 Dextrose monohydrate. (a) Dextrose monohydrate is purified and crystallized D.../mass (m/m), and the reducing sugar content (dextrose equivalent), expressed as D-glucose, is not less...

  2. Dehydration of detomidine hydrochloride monohydrate.

    Science.gov (United States)

    Veldre, K; Actiņš, A; Jaunbergs, J

    2011-10-09

    The thermodynamic stability of detomidine hydrochloride monohydrate has been evaluated on the basis of phase transition kinetics in solid state. A method free of empirical models was used for the treatment of kinetic data, and compared to several known solid state kinetic data processing methods. Phase transitions were monitored by powder X-ray diffraction (PXRD) and thermal analysis. Full PXRD profiles were used for determining the phase content instead of single reflex intensity measurements, in order to minimize the influence of particle texture. We compared the applicability of isothermal and nonisothermal methods to our investigation of detomidine hydrochlorine monohydrate dehydration. Copyright © 2011 Elsevier B.V. All rights reserved.

  3. 2-Hydroxy-1-methoxyanthraquinone monohydrate

    Directory of Open Access Journals (Sweden)

    Zhi-Meng Liu

    2009-07-01

    Full Text Available The title compound, C15H10O4·H2O, also known as alizarin 1-methyl ether monohydrate, was isolated from Morinda officinalis How. The anthraquinone ring system is almost planar, the dihedral angle between the two outer benzene rings being 3.07 (4°. In the crystal structure, O—H...O hydrogen bonds link the organic molecules and the water molecules, forming a three-dimensional network.

  4. Structure of sodium perbromate monohydrate

    International Nuclear Information System (INIS)

    Blackburn, A.C.; Gallucci, J.C.; Gerkin, R.E.; Reppart, W.J.

    1992-01-01

    NaBrO 4 .H 2 O, M r =184.90, monoclinic, C2/c, a=15.7575(19), b=5.7373(15), c=11.3390(19) A, β=111.193(10)deg. In this structure, there are two inequivalent Na ions, each coordinated by six O atoms. In each of the two types of distorted octahedra, there are three inequivalent Na-O distances; the average Na(1)-O and Na(2)-O distances are 2.379(10) and 2.405(23) A, respectively. The perbromate ion in this structure displays very nearly regular tetrahedral geometry, although it is subject to no symmetry constraints; the average observed Br-O distance is 1.601(4) A, while the average observed O-Br-O angle is 109.5(9)deg. These values agree well with previously reported values. The perbromate ion, but neither of the sodium coordination polyhedra, shows rigid-body behavior. The average rigid-body corrected Br-O distance in the perbromate ion is 1.624(3) A. Refinement of the two inequivalent H atoms permitted detailed analysis of the hydrogen bonding, which is slightly different from that reported for the isomorphic sodium perchlorate monohydrate. Dynamic disordering of the H atoms as detailed by magnetic resonance methods for sodium perchlorate monohydrate is not clearly indicated in our X-ray study of sodium perbromate monohydrate. (orig./GSCH)

  5. Sodium 2-mercaptoethanesulfonate monohydrate (coenzyme M sodium salt monohydrate

    Directory of Open Access Journals (Sweden)

    Stefan Mayr

    2008-11-01

    Full Text Available The 2-thioethanesulfonate anion is the smallest known coenzyme in nature (HS–CoM and plays a key role in methanogenesis by anaerobic archaea, as well as in the oxidation of alkenes by Gram-negative and Gram-positive eubacteria. The title compound, Na+·C2H5O3S2−·H2O, is the Na+ salt of HS–CoM crystallized as the monohydrate. Six O atoms form a distorted octahedral coordination geometry around the Na atom, at distances in the range 2.312 (4–2.517 (3 Å. Two O atoms of the sulfonate group, one O atom of each of three other symmetry-related sulfonate groups plus the water O atom form the coordination environment of the Na+ ion. This arrangement forms Na–O–Na layers in the crystal structure, parallel to (100.

  6. Induced Nanocrystallization of Dextrose Monohydrate

    Science.gov (United States)

    Johnson, Irudayaraj; Raj, B. Kanickai; Sivagami, V.; Selvi, Naga Pondy

    2013-09-01

    Modern ultrasound induction is very much useful in crystallization process. It uses piezoelectric transducers or quartz crystals to convert mechanical waves to electrical signals and vice versa. Growth of a crystal is environment dependent. The characteristics of grown crystals depend on impurities, temperature, preparation of the solution and mechanical agitation. The properties and size of a crystal can be tailored by controlling any one or all the above factors. The most interesting fact is that the ultrasound influences the properties and size of a crystal. It is found that the characteristics are improved and tailored for a specific need of the industry when a crystal is grown by radiating ultrasonic wave. In some cases, it produces nanocrystals. We used a device which generates the Ultrasonic wave of 15 MHz, which is applied to the crystal right from the time before nucleation till the crystal formation. The Dextrose monohydrate crystals are grown by conventional slow cool batch method. In the same slow cool batch method, Ultrasonic waves of 15 MHz are allowed to pass, influence the nucleation, crystal formation and growing process. The crystal formation process under the exposure of Ultrasound is allowed to continue for a sufficiently long time to yield the desired nanocrystals. The FTIR, UV, microhardness and SEM analysis are taken for the crystals with and without ultrasound.

  7. Trapping crystal nucleation of cholesterol monohydrate

    DEFF Research Database (Denmark)

    Solomonov, I.; Weygand, M.J.; Kjær, K.

    2005-01-01

    Crystalline nucleation of cholesterol at the air-water interface has been studied via grazing incidence x-ray diffraction using synchrotron radiation. The various stages of cholesterol molecular assembly from monolayer to three bilayers incorporating interleaving hydrogen-bonded water layers......, at least initially, an intralayer cholesterol rearrangement in a single-crystal-to-single-crystal transition. The preferred nucleation of the monoclinic phase of cholesterol . H2O followed by transformation to the stable monohydrate phase may be associated with an energetically more stable cholesterol...... bilayer arrangement of the former and a more favorable hydrogen-bonding arrangement of the latter. The relevance of this nucleation process of cholesterol monohydrate to pathological crystallization of cholesterol from cell biomembranes is discussed....

  8. A Search for Interstellar Monohydric Thiols

    Energy Technology Data Exchange (ETDEWEB)

    Gorai, Prasanta; Das, Ankan; Das, Amaresh; Chakrabarti, Sandip K. [Indian Centre for Space Physics, 43 Chalantika, Garia Station Rd., Kolkata, 700084 (India); Sivaraman, Bhalamurugan [Atomic Molecular and Optical Physics Division, Physical Research Laboratory, Ahmedabad, 380009 (India); Etim, Emmanuel E., E-mail: ankan.das@gmail.com [Indian Institute of Science Bangalore, 560012 (India)

    2017-02-10

    It has been pointed out by various astronomers that a very interesting relationship exists between interstellar alcohols and the corresponding thiols (sulfur analog of alcohols) as far as the spectroscopic properties and chemical abundances are concerned. Monohydric alcohols such as methanol and ethanol are widely observed and 1-propanol was recently claimed to have been seen in Orion KL. Among the monohydric thiols, methanethiol (chemical analog of methanol) has been firmly detected in Orion KL and Sgr B2(N2) and ethanethiol (chemical analog of ethanol) has been observed in Sgr B2(N2), though the confirmation of this detection is yet to come. It is very likely that higher order thiols could be observed in these regions. In this paper, we study the formation of monohydric alcohols and their thiol analogs. Based on our quantum chemical calculation and chemical modeling, we find that the Tg conformer of 1-propanethiol is a good candidate of astronomical interest. We present various spectroscopically relevant parameters of this molecule to assist in its future detection in the interstellar medium.

  9. Dehydration of sodium carbonate monohydrate with indirect microwave heating

    International Nuclear Information System (INIS)

    Seyrankaya, Abdullah; Ozalp, Baris

    2006-01-01

    In this study, dehydration of sodium carbonate monohydrate (Na 2 CO 3 .H 2 O) (SCM) in microwave (MW) field with silicon carbide (SiC) as an indirect heating medium was investigated. SCM samples containing up to 3% free moisture were placed in the microwave oven. The heating experiments showed that SCM is a poor microwave energy absorber for up to 6 min of irradiation at an 800 W of microwave power. The heat for SCM calcination is provided by SiC which absorbs microwave. The monohydrate is then converted to anhydrous sodium carbonate on the SiC plate by calcining, i.e. by removing the crystal water through heating of the monohydrate temperatures of over 120 deg. C. The calcination results in a solid phase recrystallization of the monohydrate into anhydrate. In the microwave irradiation process, dehydration of SCM in terms of indirect heating can be accelerated by increasing the microwave field power

  10. Terahertz spectroscopic investigation of gallic acid and its monohydrate

    Science.gov (United States)

    Zhang, Bo; Li, Shaoping; Wang, Chenyang; Zou, Tao; Pan, Tingting; Zhang, Jianbing; Xu, Zhou; Ren, Guanhua; Zhao, Hongwei

    2018-02-01

    The low-frequency spectra of gallic acid (GA) and its monohydrate were investigated by terahertz time-domain spectroscopy (THz-TDS) in the range of 0.5 to 4.5 THz. The dehydration process of GA monohydrate was monitored on-line. The kinetic mechanism of the dehydration process was analyzed depending on the THz spectral change at different temperatures. The results indicate that the diffusion of water molecule dominates the speed of the entire dehydration process. Solid-state density functional theory (DFT) calculations of the vibrational modes of both GA and its monohydrate were performed based on their crystalline structures for better interpreting the experimental THz spectra. The results demonstrate that the characterized features of GA mainly originate from the collective vibrations of molecules. And the interactions between GA and water molecules are responsible for THz fingerprint of GA monohydrate. Multi-techniques including differential scanning calorimetry and thermogravimetry (DSC-TG) and powder X-ray diffraction (PXRD) were also carried out to further investigate GA and its monohydrate.

  11. Preparation and properties of uranyl bromate monohydrate

    International Nuclear Information System (INIS)

    Weigel, F.

    1983-01-01

    Uranyl bromate monohydrate UO 2 (BrO 3 ) 2 .H 2 O was obtained as a greenish-yellow solid by the metathesis of a uranyl sulfate solution with a stoichiometric amount of barium bromate solution. On evaporation of the supernatant of the precipitated BaSO 4 a greenish-yellow syrup was obtained which, on dehydration with anhydrous carbon tetrachloride, yielded a free-flowing greenish-yellow powder with stoichiometry UO 2 (BrO 3 ) 2 .H 2 O. Powder diffraction diagrams of UO 2 (BrO 3 ) 2 .H 2 O obtained using the Guinier method yielded an orthorhombic lattice (space group, Pbcn (no. 60)) with a = 8.533 +- 0.003 A, b = 7.639 +- 0.003 A and c = 12.293 +- 0.004 A; the X-ray density was 4.507 g cm -3 . The compound was characterized by chemical analysis, IR spectroscopy and differential thermal analysis. (Auth.)

  12. Influence of impurities on the crystallization of dextrose monohydrate

    Science.gov (United States)

    Markande, Abhay; Nezzal, Amale; Fitzpatrick, John; Aerts, Luc; Redl, Andreas

    2012-08-01

    The effects of impurities on dextrose monohydrate crystallization were investigated. Crystal nucleation and growth kinetics in the presence of impurities were studied using an in-line focused beam reflectance monitoring (FBRM) technique and an in-line process refractometer. Experimental data were obtained from runs carried out at different impurity levels between 4 and 11 wt% in the high dextrose equivalent (DE) syrup. It was found that impurities have no significant influence on the solubility of dextrose in water. However, impurities have a clear influence on the nucleation and growth kinetics of dextrose monohydrate crystallization. Nucleation and growth rate were favored by low levels of impurities in the syrup.

  13. Effect of monohydric alcohols on structural properties of macromolecular solutions

    International Nuclear Information System (INIS)

    Giordano, R.; Wanderlingh, F.; Cordone, L.; Cupane, A.

    1983-01-01

    A report on the effects of monohydric alcohols on the thixotropic properties of a 1% (by weight) BSA solution is given. The presence of alcohols in the solution medium, even in a very small amount, weakens the structure responsible for the thixotropic properties: this effect increases with increasing alcohol concentration and alkyl group size. Indirect evidence relating the observed effects to the alteration, in the presence of alcohol, of protein-solvent hydrophobic interactions is also presented

  14. Terahertz absorption signatures of lactose monohydrate in crystalline form

    International Nuclear Information System (INIS)

    Jung, Euna; Kim, Jeonghoi; Han, Younho; Moon, Kiwon; Lim, Meehyun; Han, Haewook

    2008-01-01

    Terahertz (THz)vibrational modes of biomolecules strongly depend on intermolecular interactions, including electrostatic, Van der Waals, and hydrogen bonds. Upon both the theoretical and experimental investigation of vibrational dynamics in biomolecules that have been done, it is turned out that low frequency vibrational modes of biomolecules exist in 0.1∼3.0THz. Recent advances of THz technology have paved the way for a wide range of practical applications in physics, chemistry, and biology. THz time domain spectroscopy (TDS)is a promising technique for studying the collective vibrational modes of biomolecules and is important to understanding the relationship between their conformation and biological function. Using THz TDS a variety of biomolecules, including DNA, polysaccharides, amino acids, and proteins have been studied, indicating the THz absorption spectroscopy can be used to probe the collective vibrational modes and hence for structural and functional studies of biomolecules. The diluted material was then pressed into 1mm thick pellet with 13mm diameter using a vacuum die. The low frequency absorption signatures of solid α lactose monohydrate have been experimentally obtained in 0.1∼2.0THz. Previous study has already reported that α lactose monohydrate in crystalline form has a strong and narrow absorption signature centered at 0.530THz. In our measurement, we observed that THz spectrum of α lactose monohydrate has strong absorption peaks centered at 0.531, 1.195, and 1.38 THz

  15. (R,S-3-Carboxy-2-(isoquinolinium-2-ylpropanoate monohydrate

    Directory of Open Access Journals (Sweden)

    Vladimir Stilinović

    2010-06-01

    Full Text Available The title compound, C13H11NO4·H2O, is a monohydrate of a betaine exhibiting a positively charged N-substituted isoquinoline group and a deprotonated carboxyl group. In the crystal, molecules are connected via short O—H...O hydrogen bonds between protonated and deprotonated carboxyl groups into chains of either R or S enantiomers along [001]. These chains are additionally connected by hydrogen bonding between water molecules and the deprotonated carboxy groups of neighbouring molecules.

  16. Clarithromycin monohydrate: a synchrotron X-ray powder study

    Directory of Open Access Journals (Sweden)

    Shigeru Itai

    2012-03-01

    Full Text Available In the crystal structure of the title compound, clarithromycin (CAM monohydrate, C38H69NO13·H2O, the water molecule behaves as a proton donor and is hydrogen bonded to the hydroxy O atom of the CAM cladinose ring. The hydroxy O atom also behaves as a proton donor, forming an intermolecular hydrogen bond with one of the hydroxy groups of the 14-membered aglycone ring. The CAM molecules are linked through these hydrogen bonds into chains running parallel to the c axis.

  17. The formation of radiation defects in monohydrate of lithium sulfate

    International Nuclear Information System (INIS)

    Bahytzhan, A.B.; Zhussupov, A.A.; Kim, L.M.

    2005-01-01

    Full text: The crystals of lithium sulfate are monohydrate. At heating it pass waterless form. This crystals are represented the convenient for study of the crystal water influence on the radiation-induced processes. After irradiation in Li 2 SO 4 · H 2 O it was established the radicals SO 3 - and SO 4 - by the EPR method. The similar radiation induced centres are characteristic for the all sulphates. We established that at after irradiation by X-rays monohydrate sulphate lithium have not the absorption bands in a range 200-800 nm. It complicates study of the given systems. The dominant peak of recombination luminescence (TL) has a maximum in area 100 K. On its high-temperature wing there is 'shoulder' showing of more high-temperature and weak luminescence. At higher temperatures some very weak of TL peaks are observed. The dehydration of the samples does not essential influence for this weak TL. Because we have concentrated the basic attention only on low temperature peaks of recombination luminescence. The TL peak of a luminescence with a maximum at 100 K as a result of thermo treatment has disappeared. Dominant emission became the TL peak with a maximum at 130 K. It is necessary to note, that after dehydration the radiative sensitivity of sulphate lithium sharply has increased. Our rough estimation for this change give value almost two orders. In monohydrate the maximum of TL peak is observed at 130 K radiation by UV. This peak can be divided into two peaks with maximums at 100 K and 130 K. At an irradiation dehydrated samples by ultraviolet light the TL peaks are not observed. The given results allow connecting a luminescence at 100 K with disintegration of defects in the subsystem of crystal water. The products radiolysis of water molecules essential influence on recombination processes in sulphate subsystem. The one hand they suppress them, with another - there is a new channel of disintegration complex anions. It is established that photoconductivity of the

  18. Transformation of zinc hydroxide chloride monohydrate to crystalline zinc oxide.

    Science.gov (United States)

    Moezzi, Amir; Cortie, Michael; McDonagh, Andrew

    2016-04-25

    Thermal decomposition of layered zinc hydroxide double salts provides an interesting alternative synthesis for particles of zinc oxide. Here, we examine the sequence of changes occurring as zinc hydroxide chloride monohydrate (Zn5(OH)8Cl2·H2O) is converted to crystalline ZnO by thermal decomposition. The specific surface area of the resultant ZnO measured by BET was 1.3 m(2) g(-1). A complicating and important factor in this process is that the thermal decomposition of zinc hydroxide chloride is also accompanied by the formation of volatile zinc-containing species under certain conditions. We show that this volatile compound is anhydrous ZnCl2 and its formation is moisture dependent. Therefore, control of atmospheric moisture is an important consideration that affects the overall efficiency of ZnO production by this process.

  19. Radiation damage mechanisms in single crystals of creatine monohydrate

    International Nuclear Information System (INIS)

    Wells, J.W.; Ko, C.

    1978-01-01

    ENDOR spectroscopy is utilized to define the temperature dependent sequence of molecular fragmentation processes occuring in x-irradiated single crystals of creatine monohydrate. Two conformations of the primary reduction product =OOC--C(H 2 ) --N(CH) 3 --C(NH 2 ) 2 + are found to undergo a series of subtle changes before deamination. The resultant radical -OOC--CH 2 then induces hydrogen abstraction to form a final room temperature product - OOC--CH--N(CH 3 ) --C(NH 2 ) + . An unknown initial oxidation species is found to decarboxylate forming the radical H 2 C--N(CH 3 ) --C(NH 2 ) 2 + which, although similar to the deamination product, exists at room temperature. The stability of this species is attributed to a delocalization of spin indicated by calculation and measurement

  20. Investigation into structure and dehydration dynamic of gallic acid monohydrate: A Raman spectroscopic study.

    Science.gov (United States)

    Cai, Qiang; Xue, Jiadan; Wang, Qiqi; Du, Yong

    2018-05-02

    The dehydration process of gallic acid monohydrate was carried out by heating method and characterized using Raman spectroscopic technique. Density functional theory calculation with B3LYP function is applied to simulate optimized structures and vibrational frequencies of anhydrous gallic acid and its corresponding monohydrated form. Different vibrational modes are assigned by comparison between experimental and theoretical Raman spectra of above two polymorphs. Raman spectra show that vibrational modes of the monohydrate are distinctively different from those of anhydrous one. Meanwhile, the dynamic information about dehydration process of gallic acid monohydrate could also be observed and monitored directly with the help of Raman spectral analysis. The decay rate of the characteristic band from gallic acid monohydrate and the growth rate of anhydrous one are pretty consistent with each other. It indicates that there is no intermediate present during the dehydration process of gallic acid monohydrate. The results could offer us benchmark works for identifying both anhydrous and hydrated pharmaceutical compounds, characterizing their corresponding molecular conformation within various crystalline forms, and also providing useful information about the process of dehydration dynamic at the microscopic molecular level. Copyright © 2018 Elsevier B.V. All rights reserved.

  1. Molecular interactions in the betaine monohydrate-polyol deep eutectic solvents: Experimental and computational studies

    Science.gov (United States)

    Zahrina, Ida; Mulia, Kamarza; Yanuar, Arry; Nasikin, Mohammad

    2018-04-01

    DES (deep eutectic solvents) are a new class of ionic liquids that have excellent properties. The strength of interaction between molecules in the DES affects their properties and applications. In this work, the strength of molecular interactions between components in the betaine monohydrate salt and polyol (glycerol or/and propylene glycol) eutectic mixtures was studied by experimental and computational studies. The melting point and fusion enthalpy of the mixtures were measured using STA (Simultaneous Thermal Analyzer). The nature and strength of intermolecular interactions were observed by FT-IR and NMR spectroscopy. The molecular dynamics simulation was used to determine the number of H-bonds, percent occupancy, and radial distribution functions in the eutectic mixtures. The interaction between betaine monohydrate and polyol is following order: betaine monohydrate-glycerol-propylene glycol > betaine monohydrate-glycerol > betaine monohydrate-propylene glycol, where the latter is the eutectic mixture with the lowest stability, strength and extent of the hydrogen bonding interactions between component molecules. The presence of intra-molecular hydrogen bonding interactions, the inter-molecular hydrogen bonding interactions between betaine molecule and polyol, and also interactions between polyol and H2O of betaine monohydrate in the eutectic mixtures.

  2. Intensify dodecylamine adsorption on magnesite and dolomite surfaces by monohydric alcohols

    Science.gov (United States)

    Zhang, Hao; Liu, Wengang; Han, Cong; Wei, Dezhou

    2018-06-01

    The flotation of magnesite and dolomite were investigated with the presence of single dodecylamine (DDA) and combined mixtures of DDA and monohydric alcohols, respectively. The adsorption behavior of DDA, butanol, hexanol and octanol on the surface of the two minerals were shown by molecular dynamics simulation, and the results were corresponding with the analysis of zeta potential, measurements of the contact angle and adsorption. Flotation results indicated that part of DDA could be replaced by the three alcohols (butanol, hexanol, octanol) to get better flotation results. Molecular dynamics simulation and the results of zeta potential and contact angle measurements indicated that adsorption of DDA on mineral surfaces could be strengthened by monohydric alcohols.

  3. Anxiolytic effects of orcinol glucoside and orcinol monohydrate in mice.

    Science.gov (United States)

    Wang, Xiaohong; Li, Guiyun; Li, Peng; Huang, Linyuan; Huang, Jianmei; Zhai, Haifeng

    2015-06-01

    Anxiety is a common psychological disorder, often occurring in combination with depression, but therapeutic drugs with high efficacy and safety are lacking. Orcinol glucoside (OG) was recently found to have an antidepressive action. To study the therapeutic potential of OG and orcinol monohydrate (OM) as anxiolytic agents. Anxiolytic effects in mice were measured using the elevated plus-maze, hole-board, and open-field tests. Eight groups of mice were included in each test. Thirty minutes before each test, mice in each group received one oral administration of OG (5, 10, or 20 mg/kg), OM (2.5, 5, or 10 mg/kg), the positive control diazepam (1 or 5 mg/kg), or control vehicle. Each mouse underwent only one test. Uptake of orcinol (5 mg/kg) in the brain was qualitatively detected using the HPLC-MS method. OG (5, 10, and 20 mg/kg) and OM (2.5 and 5 mg/kg) increased the time spent in open arms and the number of entries into open arms in the elevated plus-maze test. OG (5 and 10 mg/kg) and OM (2.5 and 5 mg/kg) increased the number of head-dips in the hole-board test. At all tested doses, OG and OM did not significantly affect the locomotion of mice in the open-field test. Orcinol could be detected in the mouse brain homogenates 30 min after oral OM administration, having confirmed that OM is centrally active. The results demonstrated that OG and OM are anxiolytic agents without sedative effects, indicating their therapeutic potential for anxiety.

  4. Lithium perbromate monohydrate at 296 and 173 K

    International Nuclear Information System (INIS)

    Blackburn, A.C.; Gerkin, R.E.

    1995-01-01

    Lithium tetraoxobromate(1-) monohydrate, LiBrO 4 .H 2 O, whose perchlorate analog has not yet been described, is found to be isomorphic with NaBrO 4 .H 2 O and NaClO 4 .H 2 O. Each of the two inequivalent Li ions is coordinated by six O atoms, thus forming distorted octahedra, each of which has three inequivalent Li-O distances. At room temperature, the average Li(1)-O and Li(2)-O distances are 2.150 and 2.164 A, respectively. The perbromate ion displays very nearly regular tetrahedral geometry, although it is not subject to symmetry constraints. At 296 K the average observed Br-O distance is 1.610 (4) A and the average O-Br-O angle is 109.5 (6) , while at 173 K the corresponding values are 1.613 (4) A and 109.5 (7) . The perbromate ion shows rigid-body behavior but the lithium coordination polyhedra do not. At 296 K, the average rigid-body corrected Br-O distance in the perbromate ion is 1.624 (3) A, in excellent agreement with the corresponding value reported for NaBrO 4 .H 2 O. Refinement of the two inequivalent H atoms allowed detailed analysis of the hydrogen bonding, which is more extensive than in NaBrO 4 .H 2 O or in NaClO 4 .H 2 O. The average observed B values for the H atoms [2.9 (3) A 2 at 296 K and 2.8 (3) A 2 at 173 K] are sufficiently small to suggest that dynamic disordering of the H atoms (determined by magnetic resonance methods for NaClO 4 .H 2 O) is not significant in the title salt. (orig.)

  5. Influence of solvents on the habit modification of alpha lactose monohydrate single crystals

    Science.gov (United States)

    Parimaladevi, P.; Srinivasan, K.

    2013-02-01

    Restricted evaporation of solvent method was adopted for the growth of alpha lactose monohydrate single crystals from different solvents. The crystal habits of grown crystals were analysed. The form of crystallization was confirmed by powder x-ray diffraction analysis. Thermal behaviour of the grown crystals was studied by using differential scanning calorimetry.

  6. (R,S)-3-Carb?oxy-2-(isoquinolinium-2-yl)propanoate monohydrate

    OpenAIRE

    Stilinovi?, Vladimir; Frkanec, Leo; Kaitner, Branko

    2010-01-01

    The title compound, C13H11NO4·H2O, is a monohydrate of a betaine exhibiting a positively charged N-substituted isoquinoline group and a deprotonated carboxyl group. In the crystal, molecules are connected via short O—H...O hydrogen bonds between protonated and deprotonated carboxyl groups into chains of either R or S enantiomers along [001]. These chains are additionally connected by hydrogen bonding between water molecules and the deprotonated carboxy groups of neighbourin...

  7. Ammonium (E-3-(4-hydroxy-3-methoxyphenylprop-2-enoate monohydrate

    Directory of Open Access Journals (Sweden)

    Li-Cai Zhu

    2010-11-01

    Full Text Available In structure of the title compound ammonium ferulate monohydrate, NH4+·C10H9O4−·H2O, O—H...O and N—H...O hydrogen bonds link the ammonium cations, ferulate anions and water molecules into a three-dimensional array. The ferulate anion is approximately planar, with a maximum deviation of 0.307 (2 Å.

  8. Protective effects of regular aerobic exercise on renal tissue injury following creatine monohydrate supplementation in rats

    Directory of Open Access Journals (Sweden)

    Davoud Rahimi

    2017-01-01

    Full Text Available Creatine is one of the most common supplements for improvement of athletic performance which is used by athletes. The most important debate about creatine consumption is its adverse effect on kidneys due to increased protein load. This study was performed to evaluate the protective effects of aerobic exercise on renal tissue injury following consumption of creatine monohydrate in the rat. For this purpose, 30 male Wistar rats were randomly divided into 3 groups of 10 animals each. Group 1, as control, received only standard food. Group 2 received 5 g/kg b.w. creatine monohydrate supplement daily for 8 weeks through gavage and group 3 received creatine monohydrate supplementation in the same manner30 minutes before aerobic exercise. Aerobic exercise was performed 5 times per week on treadmill at speed of 10-25m/min for 10-30 minutes with the slope of 5 degrees. At the end of 8 weeks, water intake and urinary excretion of rats were measured and blood samples were collected for measurement of serum renal function biomarkers including urea, uric acid and creatinine. Finally, the rats were euthanized for renal histopathology. In group 3, by doing regular aerobic exercise, water intake and urinary excretion rates were significantly (p

  9. A novel quantification method of pantaprazole sodium monohydrate in sesquihydrate by thermogravimetric analyzer.

    Science.gov (United States)

    Reddy, V Ranga; Rajmohan, M Anantha; Shilpa, R Laxmi; Raut, Dilip M; Naveenkumar, Kolla; Suryanarayana, M V; Mathad, Vijayavitthal T

    2007-04-11

    To demonstrate the applicability of thermogravimetric analyzer as a tool for the quantification of pantaprazole sodium monohydrate in sesquihydrate, studies have been conducted. Thermal analysis (DSC, TGA) crystallographic (PXRD) and spectroscopic techniques (FT-IR) were used for the characterization of the polymorphs. Thermogravimetric analysis (TGA) analysis was explored by high-resolution dynamic (Hi-Res-dynamic) and high-resolution modulated (Hi-Res-modulated) test procedures to quantify the hydrate polymorphic mixtures. The two polymorphic forms exhibited significant differences and good resolution in the second derivative thermogram generated by Hi-Res-modulated test procedure. Thus, the TGA with Hi-Res-modulated test procedure was considered for the quantification of monohydrate in sesquihydrate. The calibration plot was constructed from the known mixtures of two polymorphs by plotting the peak area of the second derivative thermogram against the weight percent of monohydrate. Using this novel approach, 1 wt% limit of detection (LOD) was achieved. The polymorphic purity results, obtained by TGA in Hi-Res-modulated test procedure were found to be in good agreement with the results predicted by FT-IR and was comparable with the actual values of the known polymorphic mixtures. The Hi-Res-modulated TGA technique is very simple and easy to perform the analysis.

  10. Plasma Creatine Kinetics After Ingestion of Microencapsulated Creatine Monohydrate with Enhanced Stability in Aqueous Solutions.

    Science.gov (United States)

    Hone, Michelle; Kent, Robert M; Scotto di Palumbo, Alessandro; Bleiel, Sinead B; De Vito, Giuseppe; Egan, Brendan

    2017-07-04

    Creatine monohydrate represents one of the largest sports supplement markets. Enhancing creatine (CRE) stability in aqueous solutions, such as with microencapsulation, represents innovation potential. Ten physically active male volunteers were randomly assigned in a double-blind design to either placebo (PLA) (3-g maltodextrin; n = 5) or microencapsulated CRE (3-g creatine monohydrate; n = 5) conditions. Experimental conditions involved ingestion of the samples in a 70-mL ready-to-drink format. CRE was delivered in a novel microencapsulation matrix material consisting entirely of hydrolyzed milk protein. Three hours after ingestion, plasma creatine concentrations were unchanged during PLA, and averaged ∼45 μM. During CRE, plasma creatine concentration peaked after 30 min at 101.6 ± 14.9 μM (p creatine concentration gradually trended downwards but remained significantly elevated (∼50% above resting levels) 3 hr after ingestion. These results demonstrate that the microencapsulated form of creatine monohydrate reported herein remains bioavailable when delivered in aqueous conditions, and has potential utility in ready-to-drink formulations for creatine supplementation.

  11. Crystal structure, vibrational and DFT simulation studies of melaminium dihydrogen phosphite monohydrate

    Science.gov (United States)

    Arjunan, V.; Kalaivani, M.; Marchewka, M. K.; Mohan, S.

    2013-08-01

    The crystal structure investigations of melamine with phosphorous acid, namely melaminium dihydrogenphosphite monohydrate (C3N6H7·H2PO3·H2O) have been investigated by means of single crystal X-ray diffraction method. The title compound crystallizes in monoclinic crystal system, and the space group is P21/c with a = 10.069 Å, b = 21.592 Å, c = 12.409 Å and Z = 12. The vibrational assignments and analysis of melaminium dihydrogen phosphite monohydrate have also been performed by FTIR, FT-Raman and far-infrared spectral studies. The quantum chemical simulations were performed with DFT (B3LYP) method using 6-31G**, cc-pVTZ, and 6-311++G** basis sets to determine the energy, structural, thermodynamic parameters and vibrational frequencies of melaminium dihydrogen phosphite monohydrate. The hydrogen atom from phosphorous acid was transferred to the melamine molecule giving the singly protonated melaminium cation. The ability of ions to form spontaneous three-dimensional structure through weak Osbnd H···O and Nsbnd H···O hydrogen bonds shows notable vibrational effects.

  12. EXERCISE PERFORMANCE AND MUSCLE CONTRACTILE PROPERTIES AFTER CREATINE MONOHYDRATE SUPPLEMENTATION IN AEROBIC-ANAEROBIC TRAINING RATS

    Directory of Open Access Journals (Sweden)

    Nickolay Boyadjiev

    2007-12-01

    Full Text Available The purpose of this study was to investigate the effects of creatine monohydrate supplementation on exercise performance and contractile variables in aerobic-anaerobic training rats. Twenty 90-day-old male Sprague Dawley rats were divided into two groups - creatine (Cr and controls (K. The creatine group received creatine monohydrate as a nutritional supplement, whereas the control group was given placebo. Both groups were trained 5 days a week on a treadmill for 20 days in a mixed (aerobic-anaerobic metabolic working regimen (27 m·min-1, 15% elevation for 40 min. The exercise performance (sprint-test, contractile properties (m. tibialis anterior, oxidative enzyme activity (SDH, LDH, NADH2 in m. soleus and blood hematological and chemical variables were assessed in the groups at the end of the experiment. It was found out that creatine supplementation improved the exercise performance after 20 days of administration in a dose of 60 mg per day on the background of a mixed (aerobic-anaerobic exercise training. At the end of the trial the Cr-group demonstrated better values for the variables which characterize the contractile properties of m. tibialis anterior containing predominantly types IIA and IIB muscle fibers. On the other hand, a higher oxidative capacity was found out in m. soleus (type I muscle fibers as a result of 20-day creatine supplementation. No side effects of creatine monohydrate supplementation were assessed by the hematological and blood biochemical indices measured in this study

  13. X-ray diffraction study of polycrystalline dipalmitoylcephalin and dipalmitoyllecithin monohydrate. 1

    International Nuclear Information System (INIS)

    Foerster, G.; Doerfler, H.D.; Sackmann, H.

    1982-01-01

    Using VAND's indexing method the powder diagrams of 1,2-dipalmitoyl-DL-phosphatidyl-choline (lecithin) monohydrate were indexed in the measured angle range of 0.20 0 0 . Cephalin crystallizes monoclinically with a = 0.986 nm, b = 0.779 nm, c = 5.462 nm, β = 92.6 0 ; lecithin triclinically with a = 0.996 nm, b = 0.859 nm, c = 5.371 nm, α = 90 0 , β = 93.3 0 , γ = 91.4 0 . The results are confronted with literature data of synthetic cephalins and lecithins with a chain length of C12, C14 and C16. (author)

  14. (R,S)-3-Carb­oxy-2-(isoquinolinium-2-yl)propanoate monohydrate

    Science.gov (United States)

    Stilinović, Vladimir; Frkanec, Leo; Kaitner, Branko

    2010-01-01

    The title compound, C13H11NO4·H2O, is a monohydrate of a betaine exhibiting a positively charged N-substituted isoquino­line group and a deprotonated carboxyl group. In the crystal, mol­ecules are connected via short O—H⋯O hydrogen bonds between protonated and deprotonated carboxyl groups into chains of either R or S enanti­omers along [001]. These chains are additionally connected by hydrogen bonding between water mol­ecules and the deprotonated carb­oxy groups of neighbouring mol­ecules. PMID:21579503

  15. (R,S)-3-Carb-oxy-2-(isoquinolinium-2-yl)propanoate monohydrate.

    Science.gov (United States)

    Stilinović, Vladimir; Frkanec, Leo; Kaitner, Branko

    2010-05-22

    The title compound, C(13)H(11)NO(4)·H(2)O, is a monohydrate of a betaine exhibiting a positively charged N-substituted isoquino-line group and a deprotonated carboxyl group. In the crystal, mol-ecules are connected via short O-H⋯O hydrogen bonds between protonated and deprotonated carboxyl groups into chains of either R or S enanti-omers along [001]. These chains are additionally connected by hydrogen bonding between water mol-ecules and the deprotonated carb-oxy groups of neighbouring mol-ecules.

  16. Theoretical calculation of zero field splitting parameters of Cr{sup 3+} doped ammonium oxalate monohydrate

    Energy Technology Data Exchange (ETDEWEB)

    Kripal, Ram, E-mail: ram_kripal2001@rediffmail.com; Yadav, Awadhesh Kumar, E-mail: aky.physics@gmail.com

    2015-06-15

    Zero field splitting parameters (ZFSPs) D and E of Cr{sup 3+} ion doped ammonium oxalate monohydrate (AOM) are calculated with formula using the superposition model. The theoretically calculated ZFSPs for Cr{sup 3+} in AOM crystal are compared with the experimental value obtained by electron paramagnetic resonance (EPR). Theoretical ZFSPs are in good agreement with the experimental ones. The energy band positions of optical absorption spectra of Cr{sup 3+} in AOM crystal calculated with CFA package are in good match with the experimental values.

  17. Solution thermodynamics of creatine monohydrate in binary (water + ethanol) solvent systems at T = (278.15 to 328.15) K

    International Nuclear Information System (INIS)

    Song, Liangcheng; Wei, Lihua; Si, Tao; Guo, Huai; Yang, Chunhui

    2016-01-01

    Highlights: • The solubilities of creatine monohydrate in (ethanol + water) mixtures were investigated. • The solubility data were well correlated by Jouyban–Acree model. • Solution thermodynamic properties were calculated. • The dissolving process of creatine monohydrate in was endothermic and entropy-driven. - Abstract: In order to optimize the crystallization process of creatine monohydrate, the solubility of creatine monohydrate in the binary (water + ethanol) mixture was measured at temperatures ranging from 278.15 K to 328.15 K using the laser monitoring technique. The solubility increased with both the temperature and the mole fraction of water in the solvent mixture. The experimental solubility was well correlated by the Jouyban–Acree model, which generated a sensitive solubility surface for creatine monohydrate. Furthermore, the thermodynamic parameters of this dissolution process were also estimated. The results showed that the dissolution process of creatine monohydrate in each solvent mixture was endothermic and entropy-driven, and that the dissolution of creatine monohydrate became much easier when the mole fraction of water in the solvent mixture increased.

  18. Deacidification of palm oil using betaine monohydrate-based natural deep eutectic solvents.

    Science.gov (United States)

    Zahrina, Ida; Nasikin, Mohammad; Krisanti, Elsa; Mulia, Kamarza

    2018-02-01

    In the palm oil industry, the deacidification process is performed by steam stripping which causes the loss of most of palm oil's natural antioxidants due to high temperature. The liquid-liquid extraction process which is carried out at low temperature is preferable in order to preserve these compounds. The use of hydrated ethanol can reduce the losses of antioxidants, but the ability of this solvent to extract free fatty acids also decreases. Betaine monohydrate-based natural deep eutectic solvents (NADES) have extensive potential for this process. The selectivity of these NADES was determined to select a preferable solvent. The betaine monohydrate-glycerol NADES in a molar ratio of 1:8 was determined to be the preferred solvent with the highest selectivity. This solvent has an efficiency of palmitic acid extraction of 34.14%, and the amount of antioxidants can be preserved in the refined palm oil up to 99%. The compounds are stable during extraction. Copyright © 2017. Published by Elsevier Ltd.

  19. The impact of material attributes and process parameters on the micronisation of lactose monohydrate.

    Science.gov (United States)

    Shariare, M H; de Matas, M; York, P; Shao, Q

    2011-04-15

    Dry powder inhalers (DPIs), which are important medicines for drug delivery to the lungs, require drug particles in the respirable size range of 1-6 μm for optimal lung deposition. Drugs administered by the oral route also derive benefit from particles in this size range owing to their large surface area to volume ratio, which provides potential for rapid dissolution. Micronisation used in the production of particles, however often leads to heterogeneous product containing mechanically activated surfaces with amorphous content. This study was therefore carried out to evaluate the effect of particle properties of three grades of lactose monohydrate, with sizes above and below the brittle-ductile transition (dcrit) and their interaction with process variables on the quality of micronised material. Following an experimental design, the impact of three factors (grinding pressure, injector pressure and feed rate) on the particulate attributes of micronised powders produced from the different size grades was assessed. Processing conditions were shown to be important determinants of powder properties only for the coarsest starting material. Ultrafine material was achieved by processing finer grade feed stock below dcrit. However the resultant product was more crystalline and transformed on heating to the anhydrous state with markedly reduced onset temperature with lower energy surfaces than powders produced from larger sized starting material. Thus the propensity for micronisation of lactose monohydrate can be altered through control of starting materials and optimal settings for process variables. Copyright © 2011 Elsevier B.V. All rights reserved.

  20. Unidirectional growth and characterization of L-arginine monohydrochloride monohydrate single crystals

    International Nuclear Information System (INIS)

    Sangeetha, K.; Babu, R. Ramesh; Bhagavannarayana, G.; Ramamurthi, K.

    2011-01-01

    Highlights: → L-Arginine monohydrochloride monohydrate (LAHCl) single crystal was grown successfully by unidirectional solution growth method for the first time. → High crystalline perfection was observed for UDS grown crystal compared to CS grown crystal. → The optical transparency and mechanical stability are high for UDS grown LAHCl single crystal. → Optical birefringence measurement on this material. → The piezoelectric resonance frequencies observation - first time observation on this material. - Abstract: L-Arginine monohydrochloride monohydrate (LAHCl) single crystals were grown successfully by conventional and unidirectional solution growth methods. The crystalline perfection of grown crystals was analyzed by high-resolution X-ray diffraction. The linear optical transmittance, mechanical stability of conventional and unidirectional grown LAHCl single crystals were analyzed and compared along (0 0 1) plane. The refractive index and birefringence of LAHCl single crystals were also measured using He-Ne laser source. From the dielectric studies, piezoelectric resonance frequencies were observed in kHz frequency range for both conventional and unidirectional grown LAHCl single crystals along (0 0 1) plane.

  1. The Effects of Creatine Monohydrate on Permeability of Coronary Artery Endothelium and Level of Blood Lipoprotein in Diabetic Rats.

    Science.gov (United States)

    Rahmani, Asghar; Asadollahi, Khairollah; Soleimannejad, Kourosh; Khalighi, Zahra; Mohsenzadeh, Yosouf; Hemati, Ruhollah; Moradkhani, Atefeh; Abangah, Ghobad

    2016-09-01

    Creatine monohydrate has beneficial effects on serum glucose. This study aimed to investigate the effects of creatine on serum biochemical markers and permeability of coronary arteries among diabetic rats. 32 Wistar rats, which weighed 150-200 grams were randomly divided into 4 groups including: group I, control; group II, creatine monohydrate; group III, diabetic rats; and group IV, diabetic rats + creatine. Creatine monohydrate was applied by 400 mg/kg/daily for 5 months. Animals' weights and blood samples were taken before and after the study. Endothelial permeability rate was measured by Evans Blue method. Data were analysed by SPSS 16. At the end of fifth month, rats' weights in diabetic group under treatment with creatine, compared to those without, increased significantly (pcreatine (pcreatine compared to untreated groups, closed to the intact group (pcreatine monohydrate caused an improvement of serum biochemical markers associated with diabetes and reduced the permeability rate of coronary arteries among diabetic rats. © 2016 by the Association of Clinical Scientists, Inc.

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

    Science.gov (United States)

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

    2017-08-01

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

  3. Effects of monohydric alcohols and polyols on the thermal stability of a protein

    Energy Technology Data Exchange (ETDEWEB)

    Murakami, Shota [Graduate School of Energy Science, Kyoto University, Uji, Kyoto 611-0011 (Japan); Kinoshita, Masahiro, E-mail: kinoshit@iae.kyoto-u.ac.jp [Institute of Advanced Energy, Kyoto University, Uji, Kyoto 611-0011 (Japan)

    2016-03-28

    The thermal stability of a protein is lowered by the addition of a monohydric alcohol, and this effect becomes larger as the size of hydrophobic group in an alcohol molecule increases. By contrast, it is enhanced by the addition of a polyol possessing two or more hydroxyl groups per molecule, and this effect becomes larger as the number of hydroxyl groups increases. Here, we show that all of these experimental observations can be reproduced even in a quantitative sense by rigid-body models focused on the entropic effect originating from the translational displacement of solvent molecules. The solvent is either pure water or water-cosolvent solution. Three monohydric alcohols and five polyols are considered as cosolvents. In the rigid-body models, a protein is a fused hard spheres accounting for the polyatomic structure in the atomic detail, and the solvent is formed by hard spheres or a binary mixture of hard spheres with different diameters. The effective diameter of cosolvent molecules and the packing fractions of water and cosolvent, which are crucially important parameters, are carefully estimated using the experimental data of properties such as the density of solid crystal of cosolvent, parameters in the pertinent cosolvent-cosolvent interaction potential, and density of water-cosolvent solution. We employ the morphometric approach combined with the integral equation theory, which is best suited to the physical interpretation of the calculation result. It is argued that the degree of solvent crowding in the bulk is the key factor. When it is made more serious by the cosolvent addition, the solvent-entropy gain upon protein folding is magnified, leading to the enhanced thermal stability. When it is made less serious, the opposite is true. The mechanism of the effects of monohydric alcohols and polyols is physically the same as that of sugars. However, when the rigid-body models are employed for the effect of urea, its addition is predicted to enhance the

  4. Molecular structures and thermodynamic properties of monohydrated gaseous iodine compounds: Modelling for severe accident simulation

    Science.gov (United States)

    Sudolská, Mária; Cantrel, Laurent; Budzák, Šimon; Černušák, Ivan

    2014-03-01

    Monohydrated complexes of iodine species (I, I2, HI, and HOI) have been studied by correlated ab initio calculations. The standard enthalpies of formation, Gibbs free energy and the temperature dependence of the heat capacities at constant pressure were calculated. The values obtained have been implemented in ASTEC nuclear accident simulation software to check the thermodynamic stability of hydrated iodine compounds in the reactor coolant system and in the nuclear containment building of a pressurised water reactor during a severe accident. It can be concluded that iodine complexes are thermodynamically unstable by means of positive Gibbs free energies and would be represented by trace level concentrations in severe accident conditions; thus it is well justified to only consider pure iodine species and not hydrated forms.

  5. A second monoclinic polymorph of ethylenediammonium bis(hydrogen squarate monohydrate

    Directory of Open Access Journals (Sweden)

    Louiza Zenkhri

    2011-05-01

    Full Text Available The title compound, C2H10N22+·2HC4O4−·H2O, a new polymorph of ethylenediammonium bis(hydrogen squarate monohydrate, was synthesized by slow evaporation of an acid solution. The asymetric unit contains two hydrogen squarate anions, two half-molecules of protonated ethylenediamine arranged around a twofold axis and one water molecule. In the crystal, N—H...O and O—H...O hydrogen bonds between the hydrogen squarate anions, protonated N atoms from the amine group and water molecules lead to a three-dimensional framework. In particular, the cohesion between the squarate groups is ensured by very short intermolecular hydrogen bonds bonds. The title compound crystallized together with the previously reported polymorph [Mathew et al. (2002. J. Mol. Struct. 641, 263–279].

  6. Circular patterns of calcium oxalate monohydrate induced by defective Langmuir-Blodgett film on quartz substrates

    Energy Technology Data Exchange (ETDEWEB)

    He Jieyu [Institute of Biomineralization and Lithiasis Research, Jinan University, Guangzhou 510632 (China); Institute of Biomineralization and Lithiasis Research, Jinan University, Guangzhou 510632 (China); Ouyang Jianming [Institute of Biomineralization and Lithiasis Research, Jinan University, Guangzhou 510632 (China); Institute of Biomineralization and Lithiasis Research, Jinan University, Guangzhou 510632 (China)], E-mail: toyjm@jnu.edu.cn

    2009-01-01

    The defective Langmuir-Blodgett (LB) film of dipalmitoylphosphatidylcholine (DPPC) on quartz injured by potassium oxalate (K{sub 2}C{sub 2}O{sub 4}) was used as a model system to induce growth of calcium oxalate crystals. Atomic force microscopy (AFM) indicated that circular defective domains with a diameter of 1-200 {mu}m existed in the LB film. Scanning electron microscopy (SEM) showed circular patterns of aggregated calcium oxalate monohydrate (COM) crystallites were induced by these defective domains. It was ascribed to that the interaction between the negatively-charged oxalate ions and the phosphatidyl groups in DPPC headgroups makes the phospholipid molecules rearranged and exist in an out-of-order state in the LB film, especially at the boundaries of liquid-condensed (LC)/liquid-expanded (LE) phases, which provide much more nucleating sites for COM crystals.

  7. 1,3-Dicyclohexyl-3-[(pyridin-2-ylcarbonyl]urea monohydrate from synchrotron radiation

    Directory of Open Access Journals (Sweden)

    Solange M. S. V. Wardell

    2011-10-01

    Full Text Available The title urea derivative crystallizes as a monohydrate, C19H27N3O2·H2O. The central C3N grouping is almost planar (r.m.s. deviation = 0.0092 Å, and the amide and pyridine groups are substantially twisted out this plane [dihedral angles = 62.80 (12 and 34.98 (10°, respectively]. Supramolecular double chains propagating along the b-axis direction feature in the crystal packing whereby linear chains sustained by N—H...O hydrogen bonds formed between the amide groups are linked by helical chains of water molecules (linked by O—H...O hydrogen bonds. The H atom that participates in these water chains is disordered over two positions of equal occupancy. The double chains are connected into a two-dimensional array by C—H...O contacts and the layers stack along the a axis.

  8. Thermal, mechanical, optical and dielectric properties of piperazinium hydrogen phosphite monohydrate NLO single crystal

    Science.gov (United States)

    Rajkumar, R.; Praveen Kumar, P.

    2018-05-01

    Optical transparent crystal of piperazinium hydrogen phosphite monohydrate (PHPM) was grown by slow evaporation method. The grown crystal was characterized by single crystal X-ray diffraction analysis and the crystal belongs to monoclinic system. The functional groups present in PHPM crystal were confirmed by FTIR analysis. UV-Visible spectrum shows that the PHPM crystal is transparent in the visible region. The mechanical behavior of PHPM crystal was characterized by Vickers hardness test. Thermal stability of PHPM crystal was analyzed by thermogravimetric analysis. Dielectric studies were also carried out for the grown crystal. The third-order nonlinear parameters such as nonlinear refractive index and nonlinear absorption coefficient have been calculated using Z scan technique.

  9. In vitro and in vivo studies of creatine monohydrate supplementation to Duroc and Landrace pigs

    DEFF Research Database (Denmark)

    Young, Jette F.; Bertram, Hanne Christine; Theil, Peter Kappel

    2007-01-01

    Duroc and Landrace pigs as well as primary myotubes from these breeds were used to investigate mechanisms behind differences in their response to creatine monohydrate (CMH). Pigs were supplemented with 0, 12.5, 25 or 50g CMH/d for 5 days (n=10 per treatment and breed). Plasma levels of creatine...... increased dose-dependently in both breeds, while muscle-creatine phosphate content increased only in the Duroc pigs. (1)H NMR metabolic profiling showed a tendency towards clustering according to CMH supplementation only among Duroc pigs, revealing a stronger response compared to Landrace pigs....... The abundance of insulin-like growth factor I and myostatin mRNA was decreased by CMH supplementation while that of type 1 IGF-receptor and creatine transporter was unaffected. Protein synthesis, increased in the myotubes from both breeds, indicating protein accretion, but no effect was observed on the m...

  10. The Influence of Creatine Monohydrate on Strength and Endurance After Doing Physical Exercise With Maximum Intensity

    Directory of Open Access Journals (Sweden)

    Asrofi Shicas Nabawi

    2017-11-01

    Full Text Available The purpose of this study was: (1 to analyze the effect of creatine monohydrate to give strength after doing physical exercise with maximum intensity, towards endurance after doing physical exercise with maximum intensity, (2 to analyze the effect of non creatine monohydrate to give strength after doing physical exercise with maximum intensity, towards endurance after doing physical exercise with maximum intensity, (3 to analyze the results of the difference by administering creatine and non creatine on strength and endurance after exercise with maximum intensity. This type of research used in this research was quantitative with quasi experimental research methods. The design of this study was using pretest and posttest control group design, and data analysis was using a paired sample t-test. The process of data collection was done with the test leg muscle strength using a strength test with back and leg dynamometer, sit ups test with 1 minute sit ups, push ups test with push ups and 30 seconds with a VO2max test cosmed quart CPET during the pretest and posttest. Furthermore, the data were analyzed using SPSS 22.0 series. The results showed: (1 There was the influence of creatine administration against the strength after doing exercise with maximum intensity; (2 There was the influence of creatine administration against the group endurance after doing exercise with maximum intensity; (3 There was the influence of non creatine against the force after exercise maximum intensity; (4 There was the influence of non creatine against the group after endurance exercise maximum intensity; (5 The significant difference with the provision of non creatine and creatine from creatine group difference delta at higher against the increased strength and endurance after exercise maximum intensity. Based on the above analysis, it can be concluded that the increased strength and durability for each of the groups after being given a workout.

  11. Structural and vibrational spectral investigations of melaminium maleate monohydrate by FTIR, FT-Raman and quantum chemical calculations

    Science.gov (United States)

    Arjunan, V.; Kalaivani, M.; Marchewka, M. K.; Mohan, S.

    2013-04-01

    The structural investigations of the molecular complex of melamine with maleic acid, namely melaminium maleate monohydrate have been carried out by quantum chemical methods in addition to FTIR, FT-Raman and far-infrared spectral studies. The quantum chemical studies were performed with DFT (B3LYP) method using 6-31G**, cc-pVDZ and 6-311++G** basis sets to determine the energy, structural and thermodynamic parameters of melaminium maleate monohydrate. The hydrogen atom from maleic acid was transferred to the melamine molecule giving the singly protonated melaminium cation. The ability of ions to form spontaneous three-dimensional structure through weak Osbnd H⋯O and Nsbnd H⋯O hydrogen bonds shows notable vibrational effects.

  12. Structural and vibrational spectral investigations of melaminium maleate monohydrate by FTIR, FT-Raman and quantum chemical calculations.

    Science.gov (United States)

    Arjunan, V; Kalaivani, M; Marchewka, M K; Mohan, S

    2013-04-15

    The structural investigations of the molecular complex of melamine with maleic acid, namely melaminium maleate monohydrate have been carried out by quantum chemical methods in addition to FTIR, FT-Raman and far-infrared spectral studies. The quantum chemical studies were performed with DFT (B3LYP) method using 6-31G(**), cc-pVDZ and 6-311++G(**) basis sets to determine the energy, structural and thermodynamic parameters of melaminium maleate monohydrate. The hydrogen atom from maleic acid was transferred to the melamine molecule giving the singly protonated melaminium cation. The ability of ions to form spontaneous three-dimensional structure through weak OH···O and NH···O hydrogen bonds shows notable vibrational effects. Copyright © 2013 Elsevier B.V. All rights reserved.

  13. Electron attachment to the guanine-cytosine nucleic acid base pair and the effects of monohydration and proton transfer.

    Science.gov (United States)

    Gupta, Ashutosh; Jaeger, Heather M; Compaan, Katherine R; Schaefer, Henry F

    2012-05-17

    The guanine-cytosine (GC) radical anion and its interaction with a single water molecule is studied using ab initio and density functional methods. Z-averaged second-order perturbation theory (ZAPT2) was applied to GC radical anion for the first time. Predicted spin densities show that the radical character is localized on cytosine. The Watson-Crick monohydrated GC anion is compared to neutral GC·H2O, as well as to the proton-transferred analogue on the basis of structural and energetic properties. In all three systems, local minima are identified that correspond to water positioned in the major and minor grooves of macromolecular DNA. On the anionic surface, two novel structures have water positioned above or below the GC plane. On the neutral and anionic surfaces, the global minimum can be described as water interacting with the minor groove. These structures are predicted to have hydration energies of 9.7 and 11.8 kcal mol(-1), respectively. Upon interbase proton-transfer (PT), the anionic global minimum has water positioned in the major groove, and the hydration energy increases to 13.4 kcal mol(-1). PT GC·H2O(•-) has distonic character; the radical character resides on cytosine, while the negative charge is localized on guanine. The effects of proton transfer are further investigated through the computed adiabatic electron affinities (AEA) of GC and monohydrated GC, and the vertical detachment energies (VDE) of the corresponding anions. Monohydration increases the AEAs and VDEs by only 0.1 eV, while proton-transfer increases the VDEs substantially (0.8 eV). The molecular charge distribution of monohydrated guanine-cytosine radical anion depends heavily on interbase proton transfer.

  14. Selectivity of a heterogeneous rhodium catalyst for the carbonylation of monohydric alcohols

    Energy Technology Data Exchange (ETDEWEB)

    Christensen, B; Scurrell, M S

    1977-01-01

    Selectivity of a heterogeneous rhodium catalyst for the carbonylation of monohydric alcohols with carbon monoxide in the presence of the corresponding alkyl iodides as promotors was studied in a glass reactor at approx. 0.05:1 alcohol/carbon monoxide ratio. The 1% by wt rhodium-zeolite catalyst was prepared by immersing a Linde molecular sieve zeolite Type 13X in rhodium trichloride at 80/sup 0/C for 15 hr. Methanol was converted to methyl acetate at 433/sup 0/-513/sup 0/K with selectivites > 90% even at the highest temperatures, and dimethyl ether was by-produced. In the absence of methyl iodide, the carbonylation rate decreased drastically but the dehydration was virtually unaffected. The selectivity for ethanol carbonylation decreased from 99% at 383/sup 0/K to 6% at 523/sup 0/K due to the formation of ethylene (predominant at > 470/sup 0/K) and diethyl ether. The only product of the reaction with propan-2-ol studied at 433/sup 0/ or 473/sup 0/K was propene with 100% conversion at 473/sup 0/K. These results are consistent with the relative ease of reactant dehydration on polar catalysts. Table and 13 references.

  15. 2-(4-Hydroxyphenyl-1H-benzimidazol-3-ium chloride monohydrate

    Directory of Open Access Journals (Sweden)

    Jazmin E. González-Padilla

    2013-09-01

    Full Text Available The title molecular salt, C13H11N2O+·Cl−·H2O, crystallizes as a monohydrate. In the cation, the phenol and benzimidazole rings are almost coplanar, making a dihedral angle of 3.18 (4°. The chloride anion and benzimidazole cation are linked by two N+—H...Cl− hydrogen bonds, forming chains propagating along [010]. These chains are linked through O—H...Cl hydrogen bonds involving the water molecule and the chloride anion, which form a diamond core, giving rise to the formation of two-dimensional networks lying parallel to (10-2. Two π–π interactions involving the imidazolium ring with the benzene and phenol rings [centroid–centroid distances = 3.859 (3 and 3.602 (3 Å, respectively], contribute to this second dimension. A strong O—H...O hydrogen bond involving the water molecule and the phenol substituent on the benzimidazole unit links the networks, forming a three-dimensional structure.

  16. Absolute Oral Bioavailability of Creatine Monohydrate in Rats: Debunking a Myth.

    Science.gov (United States)

    Alraddadi, Eman A; Lillico, Ryan; Vennerstrom, Jonathan L; Lakowski, Ted M; Miller, Donald W

    2018-03-08

    Creatine is an ergogenic compound used by athletes to enhance performance. Supplementation with creatine monohydrate (CM) has been suggested for musculoskeletal and neurological disorders. Until now, little is known about its pharmacokinetic profile. Our objective was to determine the oral bioavailability of CM and the influence of dose on oral absorption. Rats were dosed orally with low dose (10 mg/kg) or high dose (70 mg/kg) 13 C-labeled CM. Blood samples were removed at various time points. Muscle and brain tissue were collected at the conclusion of the study. Plasma and tissue levels of 13 C-labeled creatine were determined using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Physiologically based pharmacokinetic (PBPK) models of CM were built using GastroPlus™. These models were used to predict the plasma concentration-time profiles of creatine hydrochloride (CHCL), which has improved aqueous solubility compared to CM. Absolute oral bioavailability for low dose CM was 53% while high dose CM was only 16%. The simulated C max of 70 mg/kg CHCL was around 35 μg/mL compared to 14 μg/mL for CM with a predicted oral bioavailability of 66% with CHCL compared to 17% with CM. Our results suggest that the oral bioavailability of CM is less than complete and subject to dose and that further examination of improved dosage formulations of creatine is warranted.

  17. High-temperature dehydration behavior and ionic conduction of 2,5-dimethylanilinium chloride monohydrate

    Energy Technology Data Exchange (ETDEWEB)

    Guidara, Sameh, E-mail: sameh_guidara@yahoo.fr; Feki, Habib; Abid, Younes

    2016-07-05

    The 2,5-dimethylanilinium chloride monohydrate compound is obtained by slow evaporation at room temperature. This material is characterized by DSC, X-Ray powder diffraction, Raman and impedance spectroscopy technique measured in the 2.10{sup 2}–5.10{sup 6} Hz frequency and 292–422 K temperature ranges. The calorimetric study has revealed three endothermic peaks at 355 K, 392 K and 403 K which defines four successive phases denoted I, II, III and IV. The first peak corresponds to water escape from the crystal. After heating above 355 K, the compound dehydrates and the crystal space group changes from non-centrosymmetric to centrosymmetric symmetry. The activation energy responsible for dielectric relaxation extracted from the modulus spectra is found to be almost the same as the value obtained from temperature variation of dc conductivity for phases I and IV. These results indicate that the transport is through ion hopping mechanism. The influence of the dehydration process on the compound conductivity was also discussed. - Highlights: • The calorimetric study of 2,5-DACM has revealed three endothermic peaks. • The dielectrical properties were studied using the impedance measurements. • The X ray powder diffraction has been performed. • The mobility of the charge carriers was reported and discussed.

  18. Fabrication and Characterizations of Hot-Melt Extruded Nanocomposites Based on Zinc Sulfate Monohydrate and Soluplus

    Directory of Open Access Journals (Sweden)

    Song Yi Lee

    2017-09-01

    Full Text Available Zinc sulfate monohydrate (ZnSO4-loaded nanocomposites (NCs were fabricated by using a hot-melt extruder (HME system. Soluplus (SP was adopted as an amphiphilic polymer matrix for HME processing. The micro-size of ZnSO4 dispersion was reduced to nano-size by HME processing with the use of SP. ZnSO4 could be homogeneously dispersed in SP through HME processing. ZnSO4/SP NCs with a 75 nm mean diameter, a 0.1 polydispersity index, and a −1 mV zeta potential value were prepared. The physicochemical properties of ZnSO4/SP NCs and the existence of SP in ZnSO4/SP NCs were further investigated by solid-state studies. Nano-size range of ZnSO4/SP NC dispersion was maintained in the simulated gastrointestinal environments (pH 1.2 and 6.8 media. No severe toxicity in intestinal epithelium after oral administration of ZnSO4/SP NCs (at 100 mg/kg dose of ZnSO4, single dosing was observed in rats. These results imply that developed ZnSO4/SP NC can be used as a promising nano-sized zinc supplement formulation. In addition, developed HME technology can be widely applied to fabricate nanoformulations of inorganic materials.

  19. Interactions between tenocytes and monosodium urate monohydrate crystals: implications for tendon involvement in gout.

    Science.gov (United States)

    Chhana, Ashika; Callon, Karen E; Dray, Michael; Pool, Bregina; Naot, Dorit; Gamble, Greg D; Coleman, Brendan; McCarthy, Geraldine; McQueen, Fiona M; Cornish, Jillian; Dalbeth, Nicola

    2014-09-01

    Advanced imaging studies have demonstrated that urate deposition in periarticular structures, such as tendons, is common in gout. The aim of this study was to investigate the effects of monosodium urate monohydrate (MSU) crystals on tenocyte viability and function. The histological appearance of tendons in joints affected by advanced gout was examined using light microscopy. In vitro, colorimetric assays and flow cytometry were used to assess cell viability in primary rat and primary human tenocytes cultured with MSU crystals. Real-time PCR was used to determine changes in the relative mRNA expression levels of tendon-related genes, and Sirius red staining was used to measure changes in collagen deposition in primary rat tenocytes. In joint samples from patients with gout, MSU crystals were identified within the tendon, adjacent to and invading into tendon, and at the enthesis. MSU crystals reduced tenocyte viability in a dose-dependent manner. MSU crystals decreased the mRNA expression of tendon collagens, matrix proteins and degradative enzymes and reduced collagen protein deposition by tenocytes. These data indicate that MSU crystals directly interact with tenocytes to reduce cell viability and function. These interactions may contribute to tendon damage in people with advanced gout. Published by the BMJ Publishing Group Limited. For permission to use (where not already granted under a licence) please go to http://group.bmj.com/group/rights-licensing/permissions.

  20. Structural, vibrational and thermal characterization of phase transformation in L-histidinium bromide monohydrate single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Moura, G.M. [Universidade Federal do Maranhão, CCSST, Imperatriz, MA, 65900-410 (Brazil); Universidade Federal do Sul e Sudeste do Pará, ICEN, Marabá, PA 68505-080 (Brazil); Carvalho, J.O. [Universidade Federal do Maranhão, CCSST, Imperatriz, MA, 65900-410 (Brazil); Instituto Federal do Tocantins, Araguaína, TO, 77.826-170 (Brazil); Silva, M.C.D.; Façanha Filho, P.F. [Universidade Federal do Maranhão, CCSST, Imperatriz, MA, 65900-410 (Brazil); Santos, A.O. dos, E-mail: adenilson1@gmail.com [Universidade Federal do Maranhão, CCSST, Imperatriz, MA, 65900-410 (Brazil)

    2015-09-01

    L-Histidinium bromide monohydrate (LHBr) single crystal is a nonlinear optical material. In this work the high temperature phase transformation and the thermal stability of single crystals of LHBr was investigated by X-ray diffraction, thermogravimetric analysis, differential thermal analysis, differential scanning calorimetry and Raman spectroscopy. The results showed the LHBr phase transformation of orthorhombic (P2{sub 1}2{sub 1}2{sub 1}) to monoclinic system (P 1 2 1) at 120 °C, with the lattice parameters a = 12.162(1) Å, b = 16.821(2) Å, c = 19.477(2) Å and β = 108.56(2)°. These techniques are complementary and confirm the structural phase transformation due to loss water of crystallization. - Highlights: • -histidinium bromide single crystal was grown by slow evaporation technique. • X-ray diffraction characterize the high-temperature phase transformation. • The structural phase transformation occur due to loss of water of crystallization. • The LHBr thermal expansion coefficients exhibit an anisotropic behavior.

  1. Design, structural investigation and physicochemical properties of benzotriazolium m-nitrophthalate monohydrate single crystals

    Science.gov (United States)

    Mekala, R.; Mani, Rajaboopathi; Jagdish, P.; Mathammal, R.

    2018-04-01

    The single crystals of organic salt benzotriazolium m-nitrophthalate monohydrate were grown by slow evaporation technique. It crystallizes in orthorhombic system with space group Pbca. The molecular interactions of the compound have been pictured using Hirshfeld surfaces and fingerprints plots and the results were compared with BZD+·mNPA-. The functional groups were identified by FTIR and FT-Raman spectra. The proton transfer from acid to base was identified from the 1H and 13C NMR spectra. The absorption and emission spectrum of BTA+·mNPA-·H2O was recorded in aqueous solution and different solvents, respectively The HOMO and LUMO energy gap of benzotriazole and BTA+·mNPA-·H2O were calculated using density functional theory (DFT). The thermal stability and melting point of hydrated salt was analysed and compared by TG-DTG/DSC study. The anti-oxidant activity of the title compound was evaluated by DPPH and ABTS+ Radical scavenging assay. The anti-microbial and anti-cancer activity showed a potential impact in the crystal.

  2. Hydrothermal synthesis, crystal structures, and enantioselective adsorption property of bis(L-histidinato)nickel(II) monohydrate

    Science.gov (United States)

    Ramos, Christian Paul L.; Conato, Marlon T.

    2018-05-01

    Despite the numerous researches in metal-organic frameworks (MOFs), there are only few reports on biologically important amino acids, histidine in particular, on its use as bridging ligand in the construction of open-framework architectures. In this work, hydrothermal synthesis was used to prepare a compound based on Ni2+ and histidine. The coordination assembly of imidazole side chain of histidine with divalent nickel ions in aqueous condition yielded purple prismatic solids. Single crystal X-ray diffraction (XRD) analysis of the product revealed structure for Ni(C6H8N3O2)2 • H2O that has a monoclinic (C2) structure with lattice parameters, a = 29.41, b = 8.27, c = 6.31 Å, β = 90.01 ˚. Circular dichroism - optical rotatory dispersion (CD-ORD), Powder X-ray diffraction (PXRD) and Fourier transform - infrared spectroscopy (FT-IR) analyses are conducted to further characterize the crystals. Enantioselective adsorption analysis using racemic mixture of 2-butanol confirmed bis(L-histidinato)nickel(II) monohydrate MOF crystal's enantioselective property preferentially favoring the adsorption of (S)-2-butanol isomer.

  3. FT-IR, FT-Raman spectra and DFT calculations of melaminium perchlorate monohydrate

    Science.gov (United States)

    Kanagathara, N.; Marchewka, M. K.; Drozd, M.; Renganathan, N. G.; Gunasekaran, S.; Anbalagan, G.

    2013-08-01

    Melaminium perchlorate monohydrate (MPM), an organic material has been synthesized by slow solvent evaporation method at room temperature. Powder X-ray diffraction analysis confirms that MPM crystal belongs to triclinic system with space group P-1. FTIR and FT Raman spectra are recorded at room temperature. Functional group assignment has been made for the melaminium cations and perchlorate anions. Vibrational spectra have also been discussed on the basis of quantum chemical density functional theory (DFT) calculations using Firefly (PC GAMESS) version 7.1 G. Vibrational frequencies are calculated and scaled values are compared with experimental values. The assignment of the bands has been made on the basis of the calculated PED. The Mulliken charges, HOMO-LUMO orbital energies are analyzed directly from Firefly program log files and graphically illustrated. HOMO-LUMO energy gap and other related molecular properties are also calculated. The theoretically constructed FT-IR and FT-Raman spectra of MPM coincide with the experimental one. The chemical structure of the compound has been established by 1H and 13C NMR spectra. No detectable signal was observed during powder test for second harmonic generation.

  4. Crystallization of calcium oxalate monohydrate at dipalmitoylphosphatidylcholine monolayers in the presence of chondroitin sulfate A

    Science.gov (United States)

    Ouyang, Jian-Ming; Deng, Sui-Ping; Zhong, Jiu-Ping; Tieke, Bernd; Yu, Shu-Hong

    2004-10-01

    The growth and aggregation of calcium oxalate monohydrate (COM) crystals beneath dipalmitoylphosphatidylcholine (DPPC) monolayers in the presence of chondroitin sulfate A (C4S) was systematically examined under different surface pressure. The results indicated that the addition of C4S can inhibit the crystal growth and prevent the aggregation of COM crystals. Under a DPPC monolayer, well-defined three-dimensional hexagonal prisms and three-dimensional rhombus prisms with sharply angled tips were obtained. The DPPC monolayer at a surface pressure of 10 mN/m can match the Ca2+ distance of the (1 bar 0 1) face of COM better than at 20 mN/m. The addition of C4S could cooperatively modulate the interaction strength between the monolayer (or itself) with the specific morphology determining faces such as (1 bar 0 1) and (0 2 0), and thus results in remarkable stabilization of the (1 bar 0 1) faces. The dramatic changes in morphological details were due to the strong electrostatic interactions between the Ca2+-rich (1 bar 0 1) crystal faces of COM and the polyanionic polysaccharide C4S together with the negatively charged sites of the zwitterionic DPPC monolayers. The increase of the concentration of C4S can further enhance the stabilization of the (1 bar 0 1) face.

  5. Preparation of Microcrystals of Piroxicam Monohydrate by Antisolvent Precipitation via Microfabricated Metallic Membranes with Ordered Pore Arrays.

    Science.gov (United States)

    Othman, Rahimah; Vladisavljević, Goran T; Simone, Elena; Nagy, Zoltan K; Holdich, Richard G

    2017-12-06

    Microcrystals of piroxicam (PRX) monohydrate with a narrow size distribution were prepared from acetone/PRX solutions by antisolvent crystallization via metallic membranes with ordered pore arrays. Crystallization was achieved by controlled addition of the feed solution through the membrane pores into a well-stirred antisolvent. A complete transformation of an anhydrous form I into a monohydrate form of PRX was confirmed by Raman spectroscopy and differential scanning calorimetry. The size of the crystals was 7-34 μm and was controlled by the PRX concentration in the feed solution (15-25 g L -1 ), antisolvent/solvent volume ratio (5-30), and type of antisolvent (Milli-Q water or 0.1-0.5 wt % aqueous solutions of hydroxypropyl methyl cellulose (HPMC), poly(vinyl alcohol) or Pluronic P-123). The smallest crystals were obtained by injecting 25 g L -1 PRX solution through a stainless-steel membrane with a pore size of 10 μm into a 0.06 wt % HPMC solution stirred at 1500 rpm using an antisolvent/solvent ratio of 20. HPMC provided better steric stabilization of microcrystals against agglomeration than poly(vinyl alcohol) and Pluronic P-123, due to hydrogen bonding interactions with PRX and water. A continuous production of large PRX monohydrate microcrystals with a volume-weighted mean diameter above 75 μm was achieved in a continuous stirred membrane crystallizer. Rapid pouring of Milli-Q water into the feed solution resulted in a mixture of highly polydispersed prism-shaped and needle-shaped crystals.

  6. Comparison of the crystal structures of the potent anticancer and anti-angiogenic agent regorafenib and its monohydrate.

    Science.gov (United States)

    Sun, Meng Ying; Wu, Su Xiang; Zhou, Xin Bo; Gu, Jian Ming; Hu, Xiu Rong

    2016-04-01

    Regorafenib {systematic name: 4-[4-({[4-chloro-3-(trifluoromethy)phenyl]carbamoyl}amino)-3-fluorophenoxy]-1-methylpyridine-2-carboxamide}, C21H15ClF4N4O3, is a potent anticancer and anti-angiogenic agent that possesses various activities on the VEGFR, PDGFR, raf and/or flt-3 kinase signaling molecules. The compound has been crystallized as polymorphic form I and as the monohydrate, C21H15ClF4N4O3·H2O. The regorafenib molecule consists of biarylurea and pyridine-2-carboxamide units linked by an ether group. A comparison of both forms shows that they differ in the relative orientation of the biarylurea and pyridine-2-carboxamide units, due to different rotations around the ether group, as measured by the C-O-C bond angles [119.5 (3)° in regorafenib and 116.10 (15)° in the monohydrate]. Meanwhile, the conformational differences are reflected in different hydrogen-bond networks. Polymorphic form I contains two intermolecular N-H...O hydrogen bonds, which link the regorafenib molecules into an infinite molecular chain along the b axis. In the monohydrate, the presence of the solvent water molecule results in more abundant hydrogen bonds. The water molecules act as donors and acceptors, forming N-H...O and O-H...O hydrogen-bond interactions. Thus, R4(2)(28) ring motifs are formed, which are fused to form continuous spiral ring motifs along the a axis. The (trifluoromethyl)phenyl rings protrude on the outside of these motifs and interdigitate with those of adjacent ring motifs, thereby forming columns populated by halogen atoms.

  7. EPR and optical absorption study of Cu{sup 2+} doped lithium sulphate monohydrate (LSMH) single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Sheela, K. Juliet; Subramanian, P., E-mail: psubramaniangri@gmail.com [Department of Physics, Gandhigram Rural Institute-Deemed University, Gandhigram, Dindigul-624302, Tamilnadu (India); Krishnan, S. Radha; Shanmugam, V. M. [CSIR-Central Electrochemical Research Institute, Karaikudi-63006, Tamilnadu (India)

    2016-05-23

    EPR study of Cu{sup 2+} doped NLO active Lithium Sulphate monohydrate (Li{sub 2}SO{sub 4.}H{sub 2}O) single crystals were grown successfully by slow evaporation method at room temperature. The principal values of g and A tensors indicate existence of orthorhombic symmetry around the Cu{sup 2+} ion. From the direction cosines of g and A tensors, the locations of Cu{sup 2+} in the lattice have been identified as interstitial site. Optical absorption confirms the rhombic symmetry and ground state wave function of the Cu{sup 2+} ion in a lattice as d{sub x2-y2}.

  8. Kidney stone matrix proteins ameliorate calcium oxalate monohydrate induced apoptotic injury to renal epithelial cells.

    Science.gov (United States)

    Narula, Shifa; Tandon, Simran; Singh, Shrawan Kumar; Tandon, Chanderdeep

    2016-11-01

    Kidney stone formation is a highly prevalent disease, affecting 8-10% of the human population worldwide. Proteins are the major constituents of human kidney stone's organic matrix and considered to play critical role in the pathogenesis of disease but their mechanism of modulation still needs to be explicated. Therefore, in this study we investigated the effect of human kidney stone matrix proteins on the calcium oxalate monohydrate (COM) mediated cellular injury. The renal epithelial cells (MDCK) were exposed to 200μg/ml COM crystals to induce injury. The effect of proteins isolated from human kidney stone was studied on COM injured cells. The alterations in cell-crystal interactions were examined by phase contrast, polarizing, fluorescence and scanning electron microscopy. Moreover, its effect on the extent of COM induced cell injury, was quantified by flow cytometric analysis. Our study indicated the antilithiatic potential of human kidney stone proteins on COM injured MDCK cells. Flow cytometric analysis and fluorescence imaging ascertained that matrix proteins decreased the extent of apoptotic injury caused by COM crystals on MDCK cells. Moreover, the electron microscopic studies of MDCK cells revealed that matrix proteins caused significant dissolution of COM crystals, indicating cytoprotection against the impact of calcium oxalate injury. The present study gives insights into the mechanism implied by urinary proteins to restrain the pathogenesis of kidney stone disease. This will provide a better understanding of the formation of kidney stones which can be useful for the proper management of the disease. Copyright © 2016 Elsevier Inc. All rights reserved.

  9. Protective Effects of Pistacia lentiscus L. fruit extract against calcium oxalate monohydrate induced proximal tubular injury.

    Science.gov (United States)

    Cheraft-Bahloul, Nassima; Husson, Cécile; Ourtioualous, Meriam; Sinaeve, Sébastien; Atmani, Djebbar; Stévigny, Caroline; Nortier, Joëlle L; Antoine, Marie-Hélène

    2017-09-14

    The world prevalence of kidney stones is increasing and plants are frequently used to treat urolithiasis. Pistacia lentiscus L, a plant which freely grows around the Mediterranean basin areas, is widely used for various pathologies. P. lentiscus has an important impact as it has economical value on top of its pharmacological interest. Decoctions of its aerial parts and/or resin are used to treat kidney stones. To in vitro assess the potential nephroprotective effect of Pistacia lentiscus ethanolic fruit extract (PLEF) on proximal tubular cells in response to the adhesion of calcium oxalate monohydrate (COM) crystals. Human Kidney [HK]-2 cells were incubated with and without COM in the presence or absence of PLEF. Cell viability was measured by the resazurin assay. The expression of E-cadherin was analyzed by PCR. The extracellular production of H 2 O 2 was measured by Amplex® Red H 2 O 2 Assay. The numbers of detached or non-adherent COM crystals in the presence of PLEF were microscopically captured and counted using ImageJ software. The interaction of PLEF with COM and the effect of PLEF on crystal size were analyzed by flow cytometry. The spectrophotometric measurement of turbidity was performed for assessing the COM concentration. PLEF incubated with COM was able to increase the cell viability. The decrease of E-cadherin expression after incubation with COM was counteracted by PLEF. Overproduction of H 2 O 2 induced by COM was also inhibited by PLEF. Observations using flow cytometry showed that interactions between PLEF and the COM crystals occurred. PLEF was also effective in reducing the particles size and in lowering COM concentration. Our data show that COM tubulotoxicity can be significantly reversed by PLEF -at least in part- via an inhibition of COM crystals adhesion onto the apical membrane. This early beneficial effect of PLEF needs to be further investigated as a useful strategy in nephrolithiasis prevention. Copyright © 2017 Elsevier Ireland Ltd

  10. Kinetic study of the dehydration reaction of lithium sulfate monohydrate crystals using microscopy and modeling

    Energy Technology Data Exchange (ETDEWEB)

    Lan, Shuiquan [Department of Mechanical Engineering, Eindhoven University of Technology, Den Dolech 2, 5612AZ Eindhoven (Netherlands); Zondag, Herbert [Department of Mechanical Engineering, Eindhoven University of Technology, Den Dolech 2, 5612AZ Eindhoven (Netherlands); Energy research Center of the Netherlands – ECN, P.O. Box 1, 1755ZG Petten (Netherlands); Steenhoven, Anton van [Department of Mechanical Engineering, Eindhoven University of Technology, Den Dolech 2, 5612AZ Eindhoven (Netherlands); Rindt, Camilo, E-mail: c.c.m.rindt@tue.nl [Department of Mechanical Engineering, Eindhoven University of Technology, Den Dolech 2, 5612AZ Eindhoven (Netherlands)

    2015-12-10

    Highlights: • Kinetics of Li{sub 2}SO{sub 4}·H{sub 2}O single crystals were modeled based on elementary processes. • Kinetics of nucleation and nuclei growth were studied by using optical microscopy. • A novel experiment was designed to visualize the reaction front into crystal bulk. • Fractional conversion was calculated and compared with TGA-experiments. - Abstract: Simulation of gas–solid reactions occurring in industrial processes requires a robust kinetic model to be applicable in a wide range of complicated reaction conditions. However, in literature it is often seen that even the same reaction under specific controlled conditions is interpreted with different kinetic models. In the present work, a phenomenological model based on nucleation and nuclei growth processes is presented to study the kinetics of the dehydration reaction of lithium sulfate monohydrate single crystals. The two elementary processes of the reaction, nucleation and nuclei growth, are characterized and quantified as a function of temperature by using optical microscopy experiments. The in-situ measured characteristics of the dehydration reaction provided confirmatory evidence that the rate of nucleation obeys an exponential law and the rate of nuclei growth is approximately constant. With knowledge acquired from the optical observations as inputs of the kinetic model, the fractional conversion of the dehydration reaction was calculated and compared with experimental results from thermogravimetric analysis (TGA). A satisfactory comparison was found both in isothermal and non-isothermal conditions. It is demonstrated that this knowledge-based model has a great potential to represent the gas–solid reaction kinetics in a wide range of process conditions regarding temperature, pressure and particle geometry.

  11. EPR and optical study of Mn{sup 2+} doped monohydrated dipotassium stannic chloride

    Energy Technology Data Exchange (ETDEWEB)

    Kripal, Ram, E-mail: ram_kripal2001@rediffmail.com; Singh, Manju

    2014-11-15

    Highlights: • EPR study of Mn{sup 2+}: DPSC crystal is done at room temperature. • The spin Hamiltonian parameters for two Mn{sup 2+} sites are determined. • The optical absorption study is also done. • The nature of metal–ligand bonding is discussed on the basis of EPR and optical data. • Theoretical zero-field splitting parameters match well with the experimental values. - Abstract: Electron paramagnetic resonance (EPR) study at room temperature (RT) is used to investigate the property of Mn{sup 2+} doped monohydrated dipotassium stannic chloride (K{sub 2}SnCl{sub 4}⋅H{sub 2}O) single crystal. EPR spectra show that there exist two substitutional sites, the spin Hamiltonian parameters for which are determined. The optical absorption study is also done at room temperature in the wavelength range 195–1100 nm. The observed bands are assigned as transitions from {sup 6}A{sub 1g}(S) ground state to various excited states. These bands are fitted with four parameters, namely Racah inter-electronic repulsion parameters B = 792 cm{sup −1}, C = 2278 cm{sup −1}; cubic crystal field splitting parameter Dq = 700 cm{sup −1} and Trees correction α = 76 cm{sup −1}. The nature of metal–ligand bonding is discussed on the basis of EPR and optical data. Superposition model (SPM) is used to find out the crystal field (CF) parameters and the perturbation formulae are used to obtain zero-field splitting (ZFS) parameters. Theoretically calculated ZFS parameters match well with the experimental values obtained from EPR study.

  12. Mimicking the biomolecular control of calcium oxalate monohydrate crystal growth: effect of contiguous glutamic acids.

    Science.gov (United States)

    Grohe, Bernd; Hug, Susanna; Langdon, Aaron; Jalkanen, Jari; Rogers, Kem A; Goldberg, Harvey A; Karttunen, Mikko; Hunter, Graeme K

    2012-08-21

    Scanning confocal interference microscopy (SCIM) and molecular dynamics (MD) simulations were used to investigate the adsorption of the synthetic polypeptide poly(l-glutamic acid) (poly-glu) to calcium oxalate monohydrate (COM) crystals and its effect on COM formation. At low concentrations (1 μg/mL), poly-glu inhibits growth most effectively in ⟨001⟩ directions, indicating strong interactions of the polypeptide with {121} crystal faces. Growth in directions was inhibited only marginally by 1 μg/mL poly-glu, while growth in directions did not appear to be affected. This suggests that, at low concentrations, poly-glu inhibits lattice-ion addition to the faces of COM in the order {121} > {010} ≥ {100}. At high concentrations (6 μg/mL), poly-glu resulted in the formation of dumbbell-shaped crystals featuring concave troughs on the {100} faces. The effects on crystal growth indicate that, at high concentrations, poly-glu interacts with the faces of COM in the order {100} > {121} > {010}. This mirrors MD simulations, which predicted that poly-glu will adsorb to a {100} terrace plane (most calcium-rich) in preference to a {121} (oblique) riser plane but will adsorb to {121} riser plane in preference to an {010} terrace plane (least calcium-rich). The effects of different poly-glu concentration on COM growth (1-6 μg/mL) may be due to variations between the faces in terms of growth mechanism and/or (nano)roughness, which can affect surface energy. In addition, 1 μg/mL might not be adequate to reach the critical concentration for poly-glu to significantly pin step movement on {100} and {010} faces. Understanding the mechanisms involved in these processes is essential for the development of agents to reduce recurrence of kidney stone disease.

  13. A study of a novel coprocessed dry binder composed of α-lactose monohydrate, microcrystalline cellulose and corn starch.

    Science.gov (United States)

    Mužíková, Jitka; Srbová, Alena; Svačinová, Petra

    2017-12-01

    This paper deals with a study of the novel coprocessed dry binder Combilac®, which contains 70% of α-lactose monohydrate, 20% of microcrystalline cellulose and 10% of native corn starch. These tests include flow properties, compressibility, lubricant sensitivity, tensile strength and disintegration time of tablets. Compressibility is evaluated by means of the energy profile of compression process, test of stress relaxation and tablet strength. The above-mentioned parameters are also evaluated in the physical mixture of α-lactose monohydrate, microcrystalline cellulose and native corn starch and compared with Combilac. Combilac shows much better flowability than the physical mixture of the used dry binders. Its compressibility is better, tablets possess a higher tensile strength. Neither Combilac, nor the physical mixture can be compressed without lubricants due to high friction and sticking to the matrix. Combilac has a higher lubricant sensitivity than the physical mixture of the dry binders. Disintegration time of Combilac tablets is comparable with the disintegration time of tablets made from the physical mixture.

  14. Solution properties and taste behavior of lactose monohydrate in aqueous ascorbic acid solutions at different temperatures: Volumetric and rheological approach.

    Science.gov (United States)

    Sarkar, Abhijit; Sinha, Biswajit

    2016-11-15

    The densities and viscosities of lactose monohydrate in aqueous ascorbic acid solutions with several molal concentrations m=(0.00-0.08)molkg(-1) of ascorbic acid were determined at T=(298.15-318.15)K and pressure p=101kPa. Using experimental data apparent molar volume (ϕV), standard partial molar volume (ϕV(0)), the slope (SV(∗)), apparent specific volumes (ϕVsp), standard isobaric partial molar expansibility (ϕE(0)) and its temperature dependence [Formula: see text] the viscosity B-coefficient and solvation number (Sn) were determined. Viscosity B-coefficients were further employed to obtain the free energies of activation of viscous flow per mole of the solvents (Δμ1(0≠)) and of the solute (Δμ2(0≠)). Effects of molality, solute structure and temperature and taste behavior were analyzed in terms of solute-solute and solute-solvent interactions; results revealed that the solutions are characterized predominantly by solute-solvent interactions and lactose monohydrate behaves as a long-range structure maker. Copyright © 2016 Elsevier Ltd. All rights reserved.

  15. CONSOLIDATION AND COMPACTION OF POWDER MIXTURES .2. BINARY-MIXTURES OF DIFFERENT PARTICLE-SIZE FRACTIONS OF ALPHA-LACTOSE MONOHYDRATE

    NARCIS (Netherlands)

    RIEPMA, KA; VEENSTRA, J; DEBOER, AH; BOLHUIS, GK; ZUURMAN, K; LERK, CF; VROMANS, H

    1991-01-01

    Binary mixtures of different particle size fractions of alpha-lactose monohydrate were compacted into tablets. The results showed decreased crushing strengths and decreased internal specific surface areas of the tablets as compared with the values calculated by linear interpolation of the data

  16. Randomized, double-blind, placebo-controlled trial of the 5-HT1A receptor antagonist AZD7371 tartrate monohydrate (robalzotan tartrate monohydrate) in patients with irritable bowel syndrome.

    Science.gov (United States)

    Drossman, Douglas A; Danilewitz, Mervyn; Naesdal, Jørgen; Hwang, Clara; Adler, John; Silberg, Debra G

    2008-10-01

    To investigate the efficacy and safety of the 5-hydroxytrypamine 1A (5-HT(1A)) receptor antagonist AZD7371 tartrate monohydrate (robalzotan tartrate monohydrate), termed AZD7371 here, in patients with irritable bowel syndrome (IBS). Patients meeting the Rome II criteria for IBS (N = 402) were randomized to treatment with AZD7371 20 mg or 5 mg or matching placebo tablets twice daily for 12 wk. The patients completed daily and weekly diary assessments, reporting abdominal discomfort or pain and description of bowel movements. They also completed validated symptom and quality-of-life questionnaires. Neither AZD7371 regimen was significantly more effective than placebo in providing adequate relief from IBS symptoms in at least 2 out of 4 wk per month over the 12 wk of treatment. There was also no significant difference between the treatment groups and placebo in the change in score in the validated symptom and quality-of-life questionnaires. Overall, 22.1% of patients experienced adverse events (AEs) attributed to the study medication: 44 of 133 (33.1%) in the 20 mg AZD7371 group, 27 of 131 (20.6%) in the 5 mg AZD7371 group, and 17 of 134 (12.7%) in the placebo group. Also, 31 of 57 (54%) of AEs leading to discontinuation were central nervous system-related. Hallucinations or hallucination-like AEs were reported by eight patients taking AZD7371, and by none of the patients in the placebo group. After these events led to discontinuation in six patients, the study was prematurely terminated. In view of the AE profile and lack of efficacy in IBS, the clinical development of AZD7371 has been stopped.

  17. Evaluation of tableting and tablet properties of Kollidon SR: the influence of moisture and mixtures with theophylline monohydrate.

    Science.gov (United States)

    Hauschild, Karsten; Picker-Freyer, Katharina M

    2006-02-01

    The aim of the study was firstly to investigate the influence of moisture on the tableting and tablet properties of Kollidon SR and secondly to investigate the influence of theophylline monohydrate on the tableting behavior and tablet properties produced from binary mixtures with Kollidon SR. In comparison to Kollidon SR, microcrystalline cellulose (MCC) was used. The glass transition temperature (Tg) of the powder over the whole range of RH (0-90%), and in addition, the Tg of tablets of Kollidon SR were measured. Densities and flowability of the powders were analyzed. The tablets were produced at five different maximum relative densities (rho(rel), max) on an instrumented eccentric tableting machine. They were produced at three different relative humidities (RH), 30%, 45%, and 60% RH for the pure substances and binary mixtures with different ratios of drug and excipient were tableted at 45% RH. The tableting properties were analyzed by 3D modeling, force-displacement profiles, and compactibility plots. First, the Tg of the powder decreased with increasing RH and the Tg of the tablet was 4-8 K lower than the powder. The predominant deformation of Kollidon SR is plastic deformation and Kollidon SR showed a higher compactibility than MCC. The parameters of the 3D model showed an extreme change between 45 and 60% RH, and at higher RH more and more particles deformed elastically. This was confirmed by analysis of force-displacement profiles. At 60% RH, the radial tensile strength of the Kollidon SR tablets was half of the radial tensile strength at 45% RH. The reason is a higher relative energy of plastic deformation than for MCC. This results in a better utilization of the energy to deform the powder into a tablet and the exceeding of the glass transition temperature at higher RH. In conclusion, at 60% RH at the same rho(rel, max), tableting and tablet properties of Kollidon SR are extremely changed since plasticity is significantly higher. In the second part of the

  18. Expanding the structural landscape of niclosamide: a high Z ' polymorph, two new solvates and monohydrate HA

    DEFF Research Database (Denmark)

    Sovago, Ioana; Bond, Andrew D.

    2015-01-01

    to be twinned by twofold rotation around that axis. The acetonitrile molecules occupy channels in the structure. A complete structure is provided for niclosamide monohydrate, C13H8Cl2N2O4·H2O, polymorph HA, obtained by Rietveld refinement against laboratory powder X-ray diffraction data. It has been suggested...... that this compound is related to the methanol solvate of niclosamide [Harriss, Wilson & Radosevljevic Evans (2014). Acta Cryst. C70, 758-763], but it is found that the two are not fully isostructural: they contain isostructural two-dimensional layers, but the layers are arranged differently in the two structures....... This suggests that HA may have the potential for polytypism, and features in the Rietveld difference curve indicate that a polytype fully isostructural with the methanol solvate might be present....

  19. Kinetic isotope effect in dehydration of ionic solids. II. The kinetics of dehydration of calcium oxalate monohydrate

    International Nuclear Information System (INIS)

    Manche, E.P.; Carroll, B.

    1977-01-01

    The kinetics of the isothermal dehydration of the protonated and deuterated monohydrate of calcium oxalate has been investigated at 120, 150, and 170 0 C. The rate of dehydration for these salts was found to be k/sub H//k/sub D/ = 1.025 +- 0.012. This result rules out the enormous kinetic isotope effect as given in the literature. An isotope effect of a few percent is not ruled out; this magnitude is in keeping with that found by Heinzinger in other dehydration processes. An estimated difference of about 150 cal/mol between the heat of desorption for H 2 O and D 2 O should have led to a ratio, k/sub h//k/sub D/ = 1.20. The smaller observed ratio has been explained on the basis of a compensation effect and may be considered an example of the Barclay--Butler correlation

  20. Setting constraints on the nature and origin of the two major hydrous sulfates on Mars: Monohydrated and polyhydrated sulfates

    Science.gov (United States)

    Wang, Alian; Jolliff, Bradley L.; Liu, Yang; Connor, Kathryn

    2016-04-01

    Monohydrated Mg sulfate (MgSO4·H2O) and polyhydrated sulfate are the most common and abundant hydrous sulfates observed thus far on Mars. They are widely distributed and coexist in many locations. On the basis of results from two new sets of experiments, in combination with past experimental studies and the subsurface salt mineralogy observed at a saline playa (Dalangtan, DLT) in a terrestrial analogue hyperarid region on the Tibet Plateau, we can now set new constraints on the nature and origin of these two major Martian sulfates. Starkeyite (MgSO4·4H2O) is the best candidate for polyhydrated sulfate. MgSO4·H2O in the form of "LH-1w," generated from dehydration of Mg sulfates with high degrees of hydration, is the most likely mineral form for the majority of Martian monohydrated Mg sulfate. Two critical properties of Mg sulfates are responsible for the coexistence of these two phases that have very different degrees of hydration: (1) the metastability of a substructural unit in starkeyite at relatively low temperatures, and (2) catalytic effects attributed to coprecipitated species (sulfates, chlorides, oxides, and hydroxides) from chemically complex brines that help overcome the metastability of starkeyite. The combination of these two properties controls the coexistence of the LH-1w layer and starkeyite layers at many locations on Mars, which sometimes occur in an interbedded stratigraphy. The structural H2O held by these two broadly distributed sulfates represents a large H2O reservoir at the surface and in the shallow subsurface on current Mars.

  1. Surfactant controlled low-temperature thermal decomposition route to zinc oxide nanorods from zinc(II) acetylacetonate monohydrate

    Energy Technology Data Exchange (ETDEWEB)

    Purkayastha, Debraj Dhar; Sarma, Bedabrat; Bhattacharjee, Chira R., E-mail: crbhattacharjee@rediffmail.com

    2014-10-15

    Zinc oxide (ZnO) nanorods were synthesized via a low-temperature thermal decomposition of zinc(II) acetylacetonate monohydrate, [Zn(C{sub 5}H{sub 7}O{sub 2}){sub 2}].H{sub 2}O. A relatively inexpensive surfactant, octadecylamine (C{sub 18}H{sub 37}NH{sub 2}) served both as a reaction solvent and a capping agent during the synthesis of ZnO nanorods. The synthesized nanorods were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), FT-IR, UV–visible, and photoluminescence (PL) studies. The XRD spectrum furnished evidence for the hexagonal wurtzite structure of ZnO. TEM images revealed the material to be rod shaped having diameter 30 nm and length 200 nm. The HRTEM image showed that the lattice fringes between the two adjacent planes are 0.244 nm apart, which corresponds to the interplanar separation of the (1 0 1) plane of hexagonal ZnO. The electron diffraction (ED) pattern confirmed the single crystalline nature of the nanorods. The PL spectrum showed two UV emissions at 356 nm (∼3.48 eV) and 382 nm (∼3.25 eV). ZnO nanorods also showed very weak blue bands at 445, 453 and 470 nm. - Highlights: Low temperature thermal decomposition of zinc(II) acetylacetonate monohydrate gave zinc oxide nanorods. Powder XRD showed hexagonal wurtzite structure of ZnO having average diameter about 24 nm. TEM images revealed the material to be of rod shape having diameter 30 nm and length 200 nm. ZnO showed band gap luminescence at 356 nm, excitonic emission at 382 nm and defect related blue bands. The synthesis is simple and can act as a paradigm for obtaining various metal oxide nanomaterials.

  2. Structural and vibrational spectral investigations of melaminium glutarate monohydrate by FTIR, FT-Raman and DFT methods

    Science.gov (United States)

    Arjunan, V.; Marchewka, M. K.; Raj, Arushma; Yang, Haifeng; Mohan, S.

    2015-01-01

    Melaminium glutarate monohydrate has been synthesised and FTIR and FT-Raman spectral investigations are carried out. The molecular geometry and vibrational frequencies of melaminium glutarate monohydrate in the ground state have been determined by using B3LYP method with 6-31++G**, 6-31++G and cc-pVDZ basis sets. The stability of the system, inter molecular hydrogen bonding and the electron donor-acceptor interactions of the complex have been investigated by using natural bonding orbital analysis. It reveals that the Nsbnd H⋯O and Osbnd H⋯O intermolecular interactions significantly influence crystal packing of this molecular complex. The glutarate anion forms hydrogen bonds to the melaminium cation as the proton donor of the type Nsbnd H⋯O with a distance (N⋯O) = 2.51 Å. It is also linked by other hydrogen bonds to the water molecule of the type Osbnd H⋯O with (O⋯O) = 2.82 Å and to the amino (sbnd NH2) group of melaminium cation of the type Nsbnd H⋯O with (N⋯O) = 2.82 Å as the proton acceptor. The electrostatic potential of the complex is in the range +1.892e × 10-2 to -1.892e × 10-2. The limits of total electron density of the complex is +6.679e × 10-2 to -6.679e × 10-2.

  3. Characterisation of 1,3-diammonium propylselenate monohydrate by XRD, FT-IR, FT-Raman, DSC and DFT studies

    Science.gov (United States)

    Thirunarayanan, S.; Arjunan, V.; Marchewka, M. K.; Mohan, S.; Atalay, Yusuf

    2016-03-01

    The crystals of 1,3-diammonium propylselenate monohydrate (DAPS) were prepared and characterised X-ray diffraction (XRD), FT-IR, FT-Raman spectroscopy, and DFT/B3LYP methods. It comprises protonated propyl ammonium moieties (diammonium propyl cations), selenate anions and water molecule which are held together by a number of hydrogen bonds and form infinite chains. The XRD data confirm the transfer of two protons from selenic acid to 1,3-diaminopropane molecule. The DAPS complex is stabilised by the presence of O-H···O and N-H···O hydrogen bonds and the electrostatic interactions as well. The N···O and O···O bond distances are 2.82-2.91 and 2.77 Å, respectively. The FT-IR and FT-Raman spectra of 1,3-diammonium propyl selenate monohydrate are recorded and the complete vibrational assignments have been discussed. The geometry is optimised by B3LYP method using 6-311G, 6-311+G and 6-311+G* basis sets and the energy, structural parameters, vibrational frequencies, IR and Raman intensities are determined. Differential scanning colorimetry (DSC) data were also presented to analyse the possibility of the phase transition. Complete natural bonding orbital (NBO) analysis is carried out to analyse the intramolecular electronic interactions and their stabilisation energies. The electrostatic potential of the complex lies in the range +1.902e × 10-2 to -1.902e × 10-2. The limits of total electron density of the complex is +8.43e × 10-2 to -8.43e × 10-2.

  4. Structural and vibrational spectral investigations of melaminium glutarate monohydrate by FTIR, FT-Raman and DFT methods.

    Science.gov (United States)

    Arjunan, V; Marchewka, M K; Raj, Arushma; Yang, Haifeng; Mohan, S

    2015-01-25

    Melaminium glutarate monohydrate has been synthesised and FTIR and FT-Raman spectral investigations are carried out. The molecular geometry and vibrational frequencies of melaminium glutarate monohydrate in the ground state have been determined by using B3LYP method with 6-31++G(**), 6-31++G and cc-pVDZ basis sets. The stability of the system, inter molecular hydrogen bonding and the electron donor-acceptor interactions of the complex have been investigated by using natural bonding orbital analysis. It reveals that the N-H⋯O and O-H⋯O intermolecular interactions significantly influence crystal packing of this molecular complex. The glutarate anion forms hydrogen bonds to the melaminium cation as the proton donor of the type N-H⋯O with a distance (N⋯O)=2.51 Å. It is also linked by other hydrogen bonds to the water molecule of the type O-H⋯O with (O⋯O)=2.82 Å and to the amino (NH2) group of melaminium cation of the type N-H⋯O with (N⋯O)=2.82 Å as the proton acceptor. The electrostatic potential of the complex is in the range +1.892e×10(-2) to -1.892e×10(-2). The limits of total electron density of the complex is +6.679e×10(-2) to -6.679e×10(-2). Copyright © 2014 Elsevier B.V. All rights reserved.

  5. Synthesis, structure and characterization of a hybrid centrosymmetric material (4-dimethylaminopyridinium nitrate gallic acid monohydrate) well-designed for non-linear optics

    Science.gov (United States)

    Ennaceur, Nasreddine; Jalel, Boutheina; Henchiri, Rokaya; Cordier, Marie; Ledoux-Rak, Isabelle

    2018-01-01

    Hybrid material: 4-Dimethylaminopyridinium nitrate gallic acid monohydrate abbreviated DNGA monohydrate has been successfully synthesized by slow evaporation method at room temperature. X-ray diffraction (XRD) on a single crystal showed that the latter was crystallized in P-1 space group. Likewise, thermal analyses demonstrated the stability of our crystal up to 80 °C. Besides, the analysis of the infrared spectrum (FTIR), allowed us to confirm the presence of the different groups present in the structure. Furthermore, by studying the UV-Visible spectrum, the transparency of our crystal was proven. Despite the fact that of having a centrosymmetric structure, the nonlinear optical properties of our single crystal, which was tested by Kurtz-Perry technique, proved that its second harmonic generation efficiency was 1.22 times more than that of KDP (potassium dihydrogen phosphate) single crystal. This nonlinear optical behavior of the studied compound was also determined through the calculations of polarizability and first hyperpolarizability values.

  6. Cognitive effects of creatine monohydrate adjunctive therapy in patients with bipolar depression: Results from a randomized, double-blind, placebo-controlled trial.

    Science.gov (United States)

    Toniolo, Ricardo Alexandre; Fernandes, Francy de Brito Ferreira; Silva, Michelle; Dias, Rodrigo da Silva; Lafer, Beny

    2017-12-15

    Depressive episodes and cognitive impairment are major causes of morbidity and dysfunction in individuals suffering from bipolar disorder (BD). Novel treatment approaches that target clinical and cognitive aspects of bipolar depression are needed, and research on pathophysiology suggests that mitochondrial modulators such as the nutraceutical creatine monohydrate might have a therapeutic role for this condition. Eighteen (N=18) patients with bipolar depression according to DSM-IV criteria who were enrollled in a 6-week, randomized, double-blind, placebo-controlled trial of creatine monohydrate 6g daily as adjunctive therapy were submitted to neuropsychological assessments (Wisconsin Card Sorting Test, Digit Span subtest of the Wechsler Adult Intelligence Scale-Third Edition, Stroop Color-Word Test, Rey-Osterrieth complex figure test, FAS Verbal Fluency Test) at baseline and week 6. There was a statistically significant difference between the treatment groups of the change on the total scores after 6 weeks in the verbal fluency test, with improvement in the group receiving adjunctive treatment with creatine. We did not find significant differences between the groups of the changes on other neuropsychological tests. Small sample and lack of a control group of healthy subjects. Our trial, which was the first to investigate the cognitive effects of creatine monohydrate on bipolar depression, indicates that supplementation with this nutraceutical for 6 weeks is associated with improvement in verbal fluency tests in patients with this condition. Copyright © 2016 Elsevier B.V. All rights reserved.

  7. Large-Scale Multifunctional Electrochromic-Energy Storage Device Based on Tungsten Trioxide Monohydrate Nanosheets and Prussian White.

    Science.gov (United States)

    Bi, Zhijie; Li, Xiaomin; Chen, Yongbo; He, Xiaoli; Xu, Xiaoke; Gao, Xiangdong

    2017-09-06

    A high-performance electrochromic-energy storage device (EESD) is developed, which successfully realizes the multifunctional combination of electrochromism and energy storage by constructing tungsten trioxide monohydrate (WO 3 ·H 2 O) nanosheets and Prussian white (PW) film as asymmetric electrodes. The EESD presents excellent electrochromic properties of broad optical modulation (61.7%), ultrafast response speed (1.84/1.95 s), and great coloration efficiency (139.4 cm 2 C -1 ). In particular, remarkable cyclic stability (sustaining 82.5% of its initial optical modulation after 2500 cycles as an electrochromic device, almost fully maintaining its capacitance after 1000 cycles as an energy storage device) is achieved. The EESD is also able to visually detect the energy storage level via reversible and fast color changes. Moreover, the EESD can be combined with commercial solar cells to constitute an intelligent operating system in the architectures, which would realize the adjustment of indoor sunlight and the improvement of physical comfort totally by the rational utilization of solar energy without additional electricity. Besides, a scaled-up EESD (10 × 11 cm 2 ) is further fabricated as a prototype. Such promising EESD shows huge potential in practically serving as electrochromic smart windows and energy storage devices.

  8. Anti-inflammatory and analgesic activity of ononitol monohydrate isolated from Cassia tora L. in animal models

    Directory of Open Access Journals (Sweden)

    Paulrayer Antonisamy

    2017-12-01

    Full Text Available Ononitol monohydrate (OM was isolated from Cassia tora L. leaves. The anti-inflammatory and analgesic activities of OM have been examined in male Wistar rats and mice. The efficacy of OM against inflammation was studied by using carrageenan-induced paw oedema, croton oil-induced ear oedema, acetic acid-induced vascular permeability, cotton pellet-induced granuloma and adjuvant-induced arthritis. The analgesic activity of OM was assessed using the acetic acid-induced abdominal constriction response, formalin-induced paw licking response and the hot-plate test. In acute type inflammation models, maximum inhibitions of 50.69 and 61.06% (P < .05 were noted with 20 mg/kg of OM in carrageenan-induced hind paw oedema and croton oil-induced ear oedema, respectively. Treatment of OM (20 mg/kg meaningfully (P < .05 reduced the granuloma tissue formation by cotton pellet study at a rate of 36.25%. OM (20 mg/kg inhibited 53.64% of paw thickness in adjuvant-induced arthritis model. OM has also been produced significant (P < .05 analgesic activity in acetic acid-induced abdominal constriction response, formalin-induced paw licking response and in hot-plate test suggesting its peripheral and central analgesic potential. The outcomes of the present study proposed that OM influenced on the anti-inflammatory and analgesic activities.

  9. A dual approach to study the electro-optical properties of a noncentrosymmetric L-asparagine monohydrate.

    Science.gov (United States)

    Shkir, Mohd; Muhammad, Shabbir; AlFaify, S; Irfan, Ahmad; Yahia, I S

    2015-02-25

    In this work we reports the experimental and theoretical investigation on an organic noncentrosymmetric monohydrated L-asparagine (LAM) molecule. LAM single crystals were grown in specially designed beaker for the first time. Structural confirmation was done by identifying the vibrational modes using IR and FT-Raman spectroscopic studies. The ultra violet-visible-near infrared absorbance, diffuse reflectance spectra were recorded in the spectral range 190-2500 nm. The optical transparency was calculated and found to be ∼80%. Its optical band gap was calculated found to be ∼5.100 eV. Density functional theory (DFT) was employed to optimize the molecular geometry of LAM using B3LYP/6-31G(∗) basis set of theory. The HOMO-LUMO energy gap of 6.047 eV and transition energy of 176 nm (f0=0.024) have been found in semi-quantitative agreement with our experimental results. The dipole moment, polarizability and first hyperpolarizability were calculated at the same level of theory. The obtained results reveals that the titled compound can be a decent contender for nonlinear applications. Copyright © 2014 Elsevier B.V. All rights reserved.

  10. Renal papillary calcification and the development of calcium oxalate monohydrate papillary renal calculi: a case series study

    Science.gov (United States)

    2013-01-01

    Background The objective of this study is to determine in a case series (four patients) how calcified deposits in renal papillae are associated with the development of calcium oxalate monohydrate (COM) papillary calculi. Methods From the recently collected papillary calculi, we evaluated retrospectively patients, subjected to retrograde ureteroscopy, with COM papillary lithiasis. Results The COM papillary calculi were found to result from subepithelial injury. Many of these lesions underwent calcification by hydroxyapatite (HAP), with calculus morphology and the amount of HAP in the concave zone dependent on the location of the calcified injury. Most of these HAP deposits grew, eroding the epithelium covering the renal papillae, coming into contact with urine and starting the development of COM calculi. Subepithelial HAP plaques may alter the epithelium covering the papillae, resulting in the deposit of COM crystals directly onto the epithelium. Tissue calcification depends on a pre-existing injury, the continuation of this process is due to modulators and/or crystallization inhibitors deficiency. Conclusions Since calculus morphology and the amount of detected HAP are dependent on the location and widespread of calcified injury, all types of papillary COM calculi can be found in the same patient. All patients had subepithelial calcifications, with fewer papillary calculi, demonstrating that some subepithelial calcifications did not further evolve and were reabsorbed. A high number of subepithelial calcifications increases the likelihood that some will be transformed into COM papillary calculi. PMID:23497010

  11. Renal papillary calcification and the development of calcium oxalate monohydrate papillary renal calculi: a case series study.

    Science.gov (United States)

    Grases, Fèlix; Costa-Bauzá, Antonia; Prieto, Rafel M; Conte, Antonio; Servera, Antonio

    2013-03-11

    The objective of this study is to determine in a case series (four patients) how calcified deposits in renal papillae are associated with the development of calcium oxalate monohydrate (COM) papillary calculi. From the recently collected papillary calculi, we evaluated retrospectively patients, subjected to retrograde ureteroscopy, with COM papillary lithiasis. The COM papillary calculi were found to result from subepithelial injury. Many of these lesions underwent calcification by hydroxyapatite (HAP), with calculus morphology and the amount of HAP in the concave zone dependent on the location of the calcified injury. Most of these HAP deposits grew, eroding the epithelium covering the renal papillae, coming into contact with urine and starting the development of COM calculi. Subepithelial HAP plaques may alter the epithelium covering the papillae, resulting in the deposit of COM crystals directly onto the epithelium. Tissue calcification depends on a pre-existing injury, the continuation of this process is due to modulators and/or crystallization inhibitors deficiency. Since calculus morphology and the amount of detected HAP are dependent on the location and widespread of calcified injury, all types of papillary COM calculi can be found in the same patient. All patients had subepithelial calcifications, with fewer papillary calculi, demonstrating that some subepithelial calcifications did not further evolve and were reabsorbed. A high number of subepithelial calcifications increases the likelihood that some will be transformed into COM papillary calculi.

  12. Role of cellular oxalate in oxalate clearance of patients with calcium oxalate monohydrate stone formation and normal controls.

    Science.gov (United States)

    Oehlschläger, Sven; Fuessel, Susanne; Meye, Axel; Herrmann, Jana; Froehner, Michael; Albrecht, Steffen; Wirth, Manfred P

    2009-03-01

    To examine the cellular, plasma, and urinary oxalate and erythrocyte oxalate flux in patients with calcium oxalate monohydrate (COM) stone formation vs normal controls. Pathologic oxalate clearance in humans is mostly integrated in calcium oxalate stone formation. An underlying cause of deficient oxalate clearance could be defective transmembrane oxalate transport, which, in many tissues, is regulated by an anion exchanger (SLC26). We studied 2 groups: 40 normal controls and 41 patients with COM stone formation. Red blood cells were divided for cellular oxalate measurement and for resuspension in a buffered solution (pH 7.40); 0.1 mmol/L oxalate was added. The supernatant was measured for oxalate immediately and 1 hour after incubation. The plasma and urinary oxalate were analyzed in parallel. The mean cellular oxalate concentrations were significantly greater in the normal controls (5.25 +/- 0.47 micromol/L) than in those with COM stone formation (2.36 +/- 0.28 micromol/L; P stone formation (0.31 +/- 0.02 mmol/L) than in the controls (0.24 +/- 0.02 mmol/L; P r = 0.49-0.63; P r = -0.29-0.41; P r = -0.30; P r = 0.25; P stone formation. Our data implicate the presence of a cellular oxalate buffer to stabilize plasma and urinary oxalate concentrations in normal controls.

  13. Experimental and theoretical investigations of non-centrosymmetric 8-hydroxyquinolinium dibenzoyl-(L)-tartrate methanol monohydrate single crystal

    International Nuclear Information System (INIS)

    Sudharsana, N.; Krishnakumar, V.; Nagalakshmi, R.

    2015-01-01

    Graphical abstract: ORTEP diagram of HQDBT. - Highlights: • Single crystal XRD and NMR studies confirm the formation of the title compound. • SHG efficiency was found to be 0.6 times that of KDP. • First-order hyperpolarizability (β) was calculated using HF and B3LYP methods. - Abstract: A novel 8-hydroxyquinolinium dibenzoyl-(L)-tartrate methanol monohydrate crystal has been grown by slow evaporation technique. The single crystal X-ray diffraction analysis has been done for the title compound and is found to crystallize in orthorhombic space group P2 1 2 1 2 1 . The optical absorption cut-off wavelength is found to be 440 nm. The vibrational analysis has been carried out to assess the functional groups present in the title compound. The molecular structure of the title compound has been confirmed by nuclear magnetic resonance spectroscopy. Thermogravimetric, differential scanning calorimetric and differential thermal analyses reveal the melting point and thermal stability of the title compound. The second harmonic generation efficiency is confirmed by Kurtz–Perry powder technique. Further quantum chemical calculations are performed using Gaussian 03 software

  14. The effects of monosodium urate monohydrate crystals on chondrocyte viability and function: implications for development of cartilage damage in gout.

    Science.gov (United States)

    Chhana, Ashika; Callon, Karen E; Pool, Bregina; Naot, Dorit; Gamble, Gregory D; Dray, Michael; Pitto, Rocco; Bentley, Jarome; McQueen, Fiona M; Cornish, Jillian; Dalbeth, Nicola

    2013-12-01

    Cartilage damage is frequently observed in advanced destructive gout. The aim of our study was to investigate the effects of monosodium urate monohydrate (MSU) crystals on chondrocyte viability and function. The alamarBlue assay and flow cytometry were used to assess the viability of primary human chondrocytes and cartilage explants following culture with MSU crystals. The number of dead chondrocytes in cartilage explants cultured with MSU crystals was quantified. Real-time PCR was used to determine changes in the relative mRNA expression levels of chondrocytic genes. The histological appearance of cartilage in joints affected by gout was also examined. MSU crystals rapidly reduced primary human chondrocyte and cartilage explant viability in a dose-dependent manner (p gout, normal cartilage architecture was lost, with empty chondrocyte lacunae observed. MSU crystals have profound inhibitory effects on chondrocyte viability and function. Interactions between MSU crystals and chondrocytes may contribute to cartilage damage in gout through reduction of chondrocyte viability and promotion of a catabolic state.

  15. Preparation and Characterization of High Purity Anhydrous β-Lactose from α-Lactose Monohydrate at Mild Temperature

    Directory of Open Access Journals (Sweden)

    Ana L. López-Pablos

    2018-01-01

    Full Text Available Lactose is a disaccharide of importance in humans dietary, food products, and the pharmaceutical industry. From the existing isomeric forms, β-lactose is rarely found in nature. Thus, in this work, a simple methodology to obtain anhydrous β-lactose (βL from α-lactose monohydrate (αL·H2O is presented. The αL·H2O powder was dispersed into a basic alcoholic solution (72 hours, at controlled conditions of temperature (27, 29, 31, and 32°C, without stirring. The slurry was dried at room temperature and characterized. Fourier transform infrared spectroscopy showed the formation of βL for the samples prepared at 29 and 32°C. Raman spectroscopy confirmed this result and suggested the occurrence of crystalline βL. Rietveld refinement of the X-ray diffraction patterns was employed to identify and quantify the composition of the isomers. The samples prepared at 29 and 31°C showed the formation of pure βL, while those at 27 and 32°C showed the presence of αL·H2O and a mixture of the two isomers, respectively. The morphology of the powders was studied by scanning electron microscopy, observing the formation of irregular shape αL·H2O particles and axe-like βL particles. Clearly, with this methodology, it was possible to obtain pure, crystalline, and anhydrous βL at mild temperature.

  16. Crystal structure of (1S,2R-2-hydroxy-1,2-diphenylethan-1-aminium (S-2-azaniumylbutanedioate monohydrate

    Directory of Open Access Journals (Sweden)

    Isao Fujii

    2017-12-01

    Full Text Available The title diastereomeric salt, formed between 2-amino-1,2-diphenylethanol (ADE and aspartic acid (ASP, C14H16NO+·C4H6NO4−·H2O, crystallizes as a monohydrate. The 1,2-diphenylethyl group in the cation has a cis conformation, and the aspartic acid anion is in the zwitterionic form. In the crystal, the ASP anions are linked via N—H...O hydrogen bonds to form a 21 helix along the b-axis direction. The helices are linked by the ADE cations via O—H...O and N—H...O hydrogen bonds, forming layers parallel to the bc plane. There are channels in the layers that are occupied by water molecules, which link to both the anions and cations via Owater—H...O and N—H...Owater hydrogen bonds. There are also C—H...O and C—H...π interactions present within the layers.

  17. Herbal extracts of Tribulus terrestris and Bergenia ligulata inhibit growth of calcium oxalate monohydrate crystals in vitro

    Science.gov (United States)

    Joshi, V. S.; Parekh, B. B.; Joshi, M. J.; Vaidya, A. B.

    2005-02-01

    A large number of people in this world are suffering from urinary stone problem. Calcium oxalate monohydrate (COM) and calcium oxalate dihydrate (COD) containing stones (calculi) are commonly found. In the present study, COM crystals were grown by a double diffusion gel growth technique using U-tubes. The gel was prepared from hydrated sodium metasilicate solution. The gel framework acts like a three-dimensional crucible in which the crystal nuclei are delicately held in the position of their formation, and nutrients are supplied for the growth. This technique can be utilized as a simplified screening static model to study the growth, inhibition and dissolution of urinary stones in vitro. The action of putative litholytic medicinal plants, Tribulus terrestris Linn. ( T.t) and Bergenia ligulata Linn. ( B.l.), has been studied in the growth of COM crystals. Tribulus terrestris and Bergenia ligulata are commonly used as herbal medicines for urinary calculi in India. To verify the inhibitive effect, aqueous extracts of Tribulus terrestris and Bergenia ligulata were added along with the supernatant solutions. The growth was measured and compared, with and without the aqueous extracts. Inhibition of COM crystal growth was observed in the herbal extracts. Maximum inhibition was observed in Bergenia ligulata followed by Tribulus terrestris. The results are discussed.

  18. Dose Optimization of Calcusol™ and Calcium Oxalate Monohydrate (COM on Primary Renal Epithelial Cells Cultures of Mice ( Mus musculus

    Directory of Open Access Journals (Sweden)

    Ahmad Soni

    2014-05-01

    Full Text Available Kidney stones are one of the urologic diseases that have plagued mankind for centuries. The main constituents of stones in the kidney are calcium oxalate monohydrate (COM crystals. Nowadays, there are varieties of drugs and treatments that can be made to minimize the grievances due to kidney stone disease. The treatment can be done either by using chemicals or traditional medicine. Calcusol™ is one of the popular herbal products that have been used by Indonesian people in curing the kidney stone disease. The main constituent that was contained in Calcusol™ is an extract of the tempuyung leaves (Sonchus arvensis L., which is expected could cure the kidney stone disease. This study used primary cultured renal epithelial cells of mice to determine the optimal dose of Calcusol™ and the optimal dose of COM. The primary Kidney epithelial cell were treated with Calcusol™ and COM at various doses. The analysis of the cell death either by necrosis or apoptosis pathways was analyzed by flow cytometric analysis. The results that were obtained is the percentage of cell death that is then analyzed by using a complete randomized design (CRD One Way Anova. Based on the results that were obtained, it is known that the optimal dose of Calcusol™ in vitro were ranging from 75 ppm to 100 ppm, whereas the optimal dose of COM suggested for 500 ppm.

  19. Validation of high performance liquid chromatographic and spectrophotometric methods for the determination of the antiparkinson agent pramipexole dihydrochloride monohydrate in pharmaceutical products

    Directory of Open Access Journals (Sweden)

    Serpil Sevim

    2015-12-01

    Full Text Available abstract The antiparkinson agent pramipexole dihydrochloride monohydrate was quantified in pharmaceutical products by high performance liquid chromatography (HPLC and derivative spectrophotometry. The first method was based on HPLC using tamsulosin HCl as an internal standard. In this method, chromatographic separation was achieved using a LiChrospher 60 RP column at 25°C, with a flow rate of 1.0 mL/min at 263 nm. The eluent comprised 0.01 mol/L ammonium acetate (pH 4.4 and acetonitrile (35:65 by volume. The linearity range was found to be 10.0-30.0 µg/mL with a mean recovery of 100.5 ± 1.10. The limit of detection (8 ng/mL and limit of quantification (50 ng/mL were calculated. In the second method, the first derivative spectrophotometric technique for the determination of pramipexole dihydrochloride monohydrate was performed by measuring the amplitude at 249 and 280 nm. In the first derivative technique, the absorbance and concentration plot was rectilinear over the 5.0-35.0 µg/mL range with a lower detection limit of 1.5 ng/mL and quantification limit of 4.5 ng/mL. The typical excipients included in the pharmaceutical product do not interfere with the selectivity of either method. The developed methods were validated for robustness, selectivity, specificity, linearity, precision, and accuracy as per the ICH and FDA guidelines (ICH Q2B, 1996; FDA,2000. In conclusion, the developed methods were successful in determining the quantity of the antiparkinson agent pramipexole dihydrochloride monohydrate in pharmaceutical products. The RSD values for the pharmaceutical product used in this study were found to be 0.97% for the HPLC method and 0.00% for the first derivative spectrophotometric method.

  20. The antitumour drug 7-ethyl-10-hydroxycamptothecin monohydrate and its solid-state hydrolysis mechanism on heating.

    Science.gov (United States)

    Ali, Md Ashraf; Noguchi, Shuji; Watanabe, Miteki; Iwao, Yasunori; Itai, Shigeru

    2016-10-01

    7-Ethyl-10-hydroxycamptothecin [systematic name: (4S)-4,11-diethyl-4,9-dihydroxy-1H-pyrano[3',4':6,7]indolizino[1,2-b]quinoline-3,14(4H,12H)-dione, SN-38] is an antitumour drug which exerts activity through the inhibition of topoisomerase I. The crystal structure of SN-38 as the monohydrate, C 22 H 20 N 2 O 5 ·H 2 O, reveals that it is a monoclinic crystal, with one SN-38 molecule and one water molecule in the asymmetric unit. When the crystal is heated to 473 K, approximately 30% of SN-38 is hydrolyzed at its lactone ring, resulting in the formation of the inactive carboxylate form. The molecular arrangement around the water molecule and the lactone ring of SN-38 in the crystal structure suggests that SN-38 is hydrolyzed by the water molecule at (x, y, z) nucleophilically attacking the carbonyl C atom of the lactone ring at (x - 1, y, z - 1). Hydrogen bonding around the water molecules and the lactone ring appears to promote this hydrolysis reaction: two carbonyl O atoms, which are hydrogen bonded as hydrogen-bond acceptors to the water molecule at (x, y, z), might enhance the nucleophilicity of this water molecule, while the water molecule at (-x, y + 1/2, -z), which is hydrogen bonded as a hydrogen-bond donor to the carbonyl O atom at (x - 1, y, z - 1), might enhance the electrophilicity of the carbonyl C atom.

  1. Qualitative and quantitative approach towards the molecular understanding of structural, vibrational and optical features of urea ninhydrin monohydrate

    Energy Technology Data Exchange (ETDEWEB)

    Sasikala, V. [Department of Physics, Bishop Moore College, Mavelikara, Alappuzha, Kerala 690110 (India); Sajan, D., E-mail: drsajanbmc@gmail.com [Department of Physics, Bishop Moore College, Mavelikara, Alappuzha, Kerala 690110 (India); Chaitanya, K. [Department of Chemistry, Nanjing University of Science and Technology, Xialingwei 200, Nanjing (China); Sundius, Tom [Department of Physics, University of Helsinki (Finland); Devi, T. Uma [Department of Physics, Government Arts College for Women (Autonomous), Pudukottai (India)

    2017-04-15

    In this study, single crystals of urea ninhydrin monohydrate (UNMH) have been grown by slow evaporation method. The grown crystals were characterized by FT-IR, FT-Raman and UV-Vis-NIR spectroscopies. The Kurtz and Perry powder method was employed to confirm the near-zero SHG efficiency of the as-grown centrosymmetric UNMH crystal. The third order nonlinearity of the crystal has been studied by the open aperture Z-scan method. The nonlinear absorption coefficient is calculated and the potentiality of UNMH in optical limiting applications is identified. The molecular geometry and the origin of optical non-linearity at the molecular level have been investigated by the density functional theory. The normal coordinate analysis was carried out to assign the molecular vibrational modes. Vibrational spectral studies confirms the presence of weak O-H⋯O and moderate O-H⋯O type hydrogen bonds in the molecule as well as O-H⋯O, N-H⋯O and blue-shifted C-H⋯O type H-bonds in the crystal. The intramolecular charge transfer interactions and the electronic absorption mechanisms have been discussed. The static and the dynamic values of hyperpolarizabilities for UNMH were estimated theoretically by DFT methods. - Highlights: • Molecular geometric and NBO interaction features of UNMH were analyzed. • Vibrational spectral features and types of H-bonding in isolated gaseous phase molecule were discussed. • Electronic absorption maxima of different phases of UNMH were found out. • The non-linear absorption behaviour of UNMH is investigated using z-scan. • First- and second- order hyperpolarizability values were estimated theoretically.

  2. Renal Epithelial Cell Injury Induced by Calcium Oxalate Monohydrate Depends on their Structural Features: Size, Surface, and Crystalline Structure.

    Science.gov (United States)

    Sun, Xin-Yuan; Ouyang, Jian-Ming; Gan, Qiong-Zhi; Liu, Ai-Jie

    2016-11-01

    Urinary crystals in normal and kidney stone patients often differ in crystal sizes and surface structures, but the effects of different crystal properties on renal tubular epithelial cells remain unclear. This study aimed to compare the cytotoxicity of micron/nano-calcium oxalate monohydrate (COM) crystals with sizes of 50 nm, 200 nm, 1 μm, 3 μm, and 10 μm to African green monkey renal epithelial (Vero) cells, to reveal the effect of crystal size and surface structure on cell injury, and to investigate the pathological mechanism of calcium oxalate kidney stones. Cell viability, cellular biochemical parameters, and internalized crystal amount in Vero cells were closely associated with the size of COM crystals. At the same concentration (200 μg/mL), COM-1 μm induced the most serious injury to Vero cells and caused the most significant change to cellular biochemical parameters, which were related to the specific porous structure and highest internalized amount in Vero cells. By contrast, COM-50 nm and COM-200 nm crystals lost their small size effect because of serious aggregation and weakened their toxicity to cells. COM-3 μm and COM-10 μm crystals were too large for cells to completely internalize; these crystals also exhibited a low specific surface area and thus weakened their toxicity. The excessive expression of intracellular ROS and reduction of the free-radical scavenger SOD were the main reasons for cell injury and eventually caused necrotic cell death. Crystal size, surface structure, aggregation, and internalization amount were closely related to the cytotoxicity of COM crystals.

  3. Monosodium urate monohydrate crystals inhibit osteoblast viability and function: implications for development of bone erosion in gout.

    Science.gov (United States)

    Chhana, Ashika; Callon, Karen E; Pool, Bregina; Naot, Dorit; Watson, Maureen; Gamble, Greg D; McQueen, Fiona M; Cornish, Jillian; Dalbeth, Nicola

    2011-09-01

    Bone erosion is a common manifestation of chronic tophaceous gout. To investigate the effects of monosodium urate monohydrate (MSU) crystals on osteoblast viability and function. The MTT assay and flow cytometry were used to assess osteoblast cell viability in the MC3T3-E1 and ST2 osteoblast-like cell lines, and primary rat and primary human osteoblasts cultured with MSU crystals. Quantitative real-time PCR and von Kossa stained mineralised bone formation assays were used to assess the effects of MSU crystals on osteoblast differentiation using MC3T3-E1 cells. The numbers of osteoblasts and bone lining cells were quantified in bone samples from patients with gout. MSU crystals rapidly reduced viability in all cell types in a dose-dependent manner. The inhibitory effect on cell viability was independent of crystal phagocytosis and was not influenced by differing crystal length or addition of serum. Long-term culture of MC3T3-E1 cells with MSU crystals showed a reduction in mineralisation and decreased mRNA expression of genes related to osteoblast differentiation such as Runx2, Sp7 (osterix), Ibsp (bone sialoprotein), and Bglap (osteocalcin). Fewer osteoblast and lining cells were present on bone directly adjacent to gouty tophus than bone unaffected by tophus in patients with gout. MSU crystals have profound inhibitory effects on osteoblast viability and differentiation. These data suggest that bone erosion in gout occurs at the tophus-bone interface through alteration of physiological bone turnover, with both excessive osteoclast formation, and reduced osteoblast differentiation from mesenchymal stem cells.

  4. Effects of Creatine Monohydrate Augmentation on Brain Metabolic and Network Outcome Measures in Women With Major Depressive Disorder.

    Science.gov (United States)

    Yoon, Sujung; Kim, Jieun E; Hwang, Jaeuk; Kim, Tae-Suk; Kang, Hee Jin; Namgung, Eun; Ban, Soonhyun; Oh, Subin; Yang, Jeongwon; Renshaw, Perry F; Lyoo, In Kyoon

    2016-09-15

    Creatine monohydrate (creatine) augmentation has the potential to accelerate the clinical responses to and enhance the overall efficacy of selective serotonin reuptake inhibitor treatment in women with major depressive disorder (MDD). Although it has been suggested that creatine augmentation may involve the restoration of brain energy metabolism, the mechanisms underlying its antidepressant efficacy are unknown. In a randomized, double-blind, placebo-controlled trial, 52 women with MDD were assigned to receive either creatine augmentation or placebo augmentation of escitalopram; 34 subjects participated in multimodal neuroimaging assessments at baseline and week 8. Age-matched healthy women (n = 39) were also assessed twice at the same intervals. Metabolic and network outcomes were measured for changes in prefrontal N-acetylaspartate and changes in rich club hub connections of the structural brain network using proton magnetic resonance spectroscopy and diffusion tensor imaging, respectively. We found MDD-related metabolic and network dysfunction at baseline. Improvement in depressive symptoms was greater in patients receiving creatine augmentation relative to placebo augmentation. After 8 weeks of treatment, prefrontal N-acetylaspartate levels increased significantly in the creatine augmentation group compared with the placebo augmentation group. Increment in rich club hub connections was also greater in the creatine augmentation group than in the placebo augmentation group. N-acetylaspartate levels and rich club connections increased after creatine augmentation of selective serotonin reuptake inhibitor treatment. Effects of creatine administration on brain energy metabolism and network organization may partly underlie its efficacy in treating women with MDD. Copyright © 2016 Society of Biological Psychiatry. Published by Elsevier Inc. All rights reserved.

  5. Engagement of fatty acids with Toll-like receptor 2 drives interleukin-1beta production via the ASC/caspase 1 pathway in monosodium urate monohydrate crystal-induced gouty arthritis.

    NARCIS (Netherlands)

    Joosten, L.A.B.; Netea, M.G.; Mylona, E.; Koenders, M.I.; Malireddi, R.K.; Oosting, M.; Stienstra, R.; Veerdonk, F.L. van de; Stalenhoef, A.F.H.; Giamarellos-Bourboulis, E.J.; Kanneganti, T.D.; Meer, J.W.M. van der

    2010-01-01

    OBJECTIVE: The concept that intraarticular crystals of uric acid by themselves trigger episodes of painful gouty arthritis is inconsistent with the clinical reality. Patients with large deposits of monosodium urate monohydrate (MSU) crystals (tophi) do not necessarily experience gouty attacks. In

  6. Bulk crystal growth and nonlinear optical characterization of semiorganic single crystal: Cadmium (II) dibromide L - Proline monohydrate

    Energy Technology Data Exchange (ETDEWEB)

    Balakrishnan, T., E-mail: balacrystalgrowth@gmail.com [Crystal Growth Laboratory, PG & Research Department of Physics, Periyar EVR College (Autonomous), Tiruchirappalli, 620 023, Tamil Nadu (India); Sathiskumar, S. [Crystal Growth Laboratory, PG & Research Department of Physics, Periyar EVR College (Autonomous), Tiruchirappalli, 620 023, Tamil Nadu (India); Ramamurthi, K. [Crystal Growth and Thin Film Laboratory, Department of Physics and Nanotechnology, SRM University, Kattankulathur, 603 203, Kancheepuram, Tamil Nadu (India); Thamotharan, S. [Department of Bioinformatics, School of Chemical and Biotechnology, SASTRA University, Thanjavur, 613 401 (India)

    2017-01-15

    Single crystal of a novel metal organic nonlinear optical (NLO) cadmium (II) dibromide L - proline monohydrate (CBLPM) of size 7 × 7 × 5 mm{sup 3} was grown from slow evaporation technique. Single crystal X – ray diffraction analysis reveals that the crystal belongs to orthorhombic system with lattice parameters a = 10.1891 (8) Å, b = 13.4961 (11) Å, c = 7.4491 (5) Å and space group P2{sub 1}2{sub 1}2{sub 1}. The powder X – ray diffraction pattern of CBLPM was recorded and the X – ray diffraction peaks were indexed. The various functional groups of CBLPM were identified by the FT – IR and FT – Raman spectral analyses. The optical transmittance window and lower cut off wavelength of CBLPM were identified from UV – Vis – NIR studies. The mechanical strength of the grown crystal was estimated using Vickers microhardness test. Dielectric constant and dielectric loss measurements were carried out at different temperatures in the frequency range of 50 Hz - 2 MHz. The photoluminescence spectrum was recorded in the wavelength range 200–400 nm and the estimated optical band gap was ∼4.1 eV. Etching studies were carried out for different etching time. Thermal stability of CBLPM was determined using thermogravimetric analysis. Laser induced damage threshold study was carried out for the grown crystal using Nd:YAG laser. Size dependent second harmonic generation efficiency of the grown crystal was determined by Kurtz and Perry powder technique with different particle size using Nd:YAG laser with wavelength 1064 nm. Second harmonic generation efficiency of the powdered CBLPM crystal was ∼2.3 times that of potassium dihydrogen orthophosphate. - Highlights: • CBLPM crystal belongs to orthorhombic crystal system with space group P2{sub 1}2{sub 1}2{sub 1.} • Transmittance of CBLPM is ∼80% in the 650–1100 nm range. • Powder SHG efficiency of CBLPM increases with increase in particle size. • SHG efficiency of 0.57 μm size powdered CBLPM is ∼2

  7. Clinical development of galunisertib (LY2157299 monohydrate, a small molecule inhibitor of transforming growth factor-beta signaling pathway

    Directory of Open Access Journals (Sweden)

    Herbertz S

    2015-08-01

    Full Text Available Stephan Herbertz,1 J Scott Sawyer,2 Anja J Stauber,2 Ivelina Gueorguieva,3 Kyla E Driscoll,4 Shawn T Estrem,2 Ann L Cleverly,3 Durisala Desaiah,2 Susan C Guba,2 Karim A Benhadji,2 Christopher A Slapak,2 Michael M Lahn21Lilly Deutschland GmbH, Bad Homburg, Germany; 2Lilly Research Laboratories, Eli Lilly and Company, Indianapolis, IN, USA; 3Lilly Research Laboratories, Eli Lilly and Company, Windlesham, Surrey, UK; 4Lilly Research Laboratories, Eli Lilly and Company, New York, NY, USA Abstract: Transforming growth factor-beta (TGF-β signaling regulates a wide range of biological processes. TGF-β plays an important role in tumorigenesis and contributes to the hallmarks of cancer, including tumor proliferation, invasion and metastasis, inflammation, angiogenesis, and escape of immune surveillance. There are several pharmacological approaches to block TGF-β signaling, such as monoclonal antibodies, vaccines, antisense oligonucleotides, and small molecule inhibitors. Galunisertib (LY2157299 monohydrate is an oral small molecule inhibitor of the TGF-β receptor I kinase that specifically downregulates the phosphorylation of SMAD2, abrogating activation of the canonical pathway. Furthermore, galunisertib has antitumor activity in tumor-bearing animal models such as breast, colon, lung cancers, and hepatocellular carcinoma. Continuous long-term exposure to galunisertib caused cardiac toxicities in animals requiring adoption of a pharmacokinetic/pharmacodynamic-based dosing strategy to allow further development. The use of such a pharmacokinetic/pharmacodynamic model defined a therapeutic window with an appropriate safety profile that enabled the clinical investigation of galunisertib. These efforts resulted in an intermittent dosing regimen (14 days on/14 days off, on a 28-day cycle of galunisertib for all ongoing trials. Galunisertib is being investigated either as monotherapy or in combination with standard antitumor regimens (including nivolumab

  8. Study of Paramagnetic Monohydrates MeSO4.1H2O (Me = Mn2+, Co2+, Fe2+, Ni2+, Cu2+

    Directory of Open Access Journals (Sweden)

    Jelšovská Kamila

    2000-09-01

    Full Text Available Nuclear magnetic resonance (NMR of protons of crystrallization water in isomorphous paramagnetic monohydrates MeSO4.1H2O with Me = Mn2+ , Co2+ , Fe2+ , Ni2+ , Cu2+ is studied in the present paper. Several physically important parameters characterizing the studied substances were derived from the NMR spectra. In this paper we analysed the dependences of the NMR second moment M2 on the magnitude of the external magnetic field induction Br and the temperature. The proton NMR spectra in paramagnetic hydrates have an asymmetric form caused by the anisotropy of the local magnetic field acting on resonating nuclei and their second moments, M2, depend linearly on the square of the external magnetic field Br. The parameters M20 (the part of the second moment M2 which corresponds to the nuclear dipole-dipole interactions and á which characterize nuclear dipole-dipole interactions of protons and paramagnetic ions, respectively, are derived from experimentally obtained dependences of M2 vs Br2. The measurements were performed at the room temperature. Calculations were realized using the approximation where two nearest neighbour ions Me2+ to each water molecule are considered. The temperature dependence of the second moment, which was realised in the temperature range 123-313 K, was more informative than the field one. Besides the individual dependences M2(T measured at fr1 and fr2 we analysed the temperature dependence of the difference ∆M2(T. Beside the second moment M20 the Curie-Weiss constant è and the magnetic moment µi of paramagnetic ions were determined from the temperature dependences. The parameters è and M20 were determined directly from the experimental data. Some knowledge on the crystalline structure for the studied substance was required for the calculation of the magnetic moment µi. By means of the classification of substances according to the Curie-Weiss parameter, the negative value of the temperature parameter è for all studied

  9. Preparation, crystal structure, vibrational spectral and density functional studies of bis (4-nitrophenol)-2,4,6-triamino-1,3,5-triazine monohydrate

    Science.gov (United States)

    Kanagathara, N.; Marchewka, M. K.; Drozd, M.; Renganathan, N. G.; Gunasekaran, S.; Anbalagan, G.

    2013-10-01

    An organic-organic salt, bis (4-nitrophenol) 2,4,6-triamino 1,3,5-triazine monohydrate (BNPM) has been prepared by slow evaporation technique at room temperature. Single crystal X-ray diffraction analysis reveals that the compound crystallizes in triclinic system with centrosymmetric space group P-1. IR and Raman spectra of BNPM have been recorded and analyzed. The study has been extended to confocal Raman spectral analysis. Band assignments have been made for the melamine and p-nitrophenol molecules. Vibrational spectra have also been discussed on the basis of quantum chemical density functional theory calculations using Firefly (PC GAMESS) Version 7.1 G. Vibrational frequencies are calculated and scaled values are compared with the experimental one. The Mulliken charges, HOMO-LUMO orbital energies are calculated and analyzed. The chemical structure of the compound was established by 1H NMR and 13C NMR spectra.

  10. Ammonium sodium fluorotrioxophosphate monohydrate

    Czech Academy of Sciences Publication Activity Database

    Fábry, Jan; Dušek, Michal; Krupková, Radmila

    2007-01-01

    Roč. 63, - (2007), i92-i94 ISSN 1600-5368 R&D Projects: GA ČR GA202/05/0421 Institutional research plan: CEZ:AV0Z10100520; CEZ:AV0Z10100521 Keywords : x-ray structure determination * O-H_O, N-H_O hydrogen bonds * fluorotrioxophosphate Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.508, year: 2007

  11. Dipotassium hydrogencarbonate fluoride monohydrate

    Directory of Open Access Journals (Sweden)

    Volker Kahlenberg

    2013-04-01

    Full Text Available Single crystals of the title compound, K2(HCO3F·H2O, were obtained as a secondary product after performing flux synthesis experiments aimed at the preparation of potassium rare earth silicates. The basic building unit of the structure is an [(HCO3(H2OF]2− zigzag chain running parallel to [001]. Both types of anions as well as the water molecules reside on mirror planes perpendicular to [010] at y = 0.25 and y = 0.75, respectively. Linkage between the different constituents of the chains is provided by O—H...O and O—H...F hydrogen bonding. The K+ cations are located between the chains and are coordinated by two F and five O atoms in form of a distorted monocapped trigonal prism.

  12. Diimidazolium phthalate monohydrate

    Directory of Open Access Journals (Sweden)

    Chua-Hua Yu

    2012-07-01

    Full Text Available In the title compound, 2C3H5N2+·C8H4O42−·H2O, the cations, anion and water molecule are connected by N—H...O and O—H...O hydrogen bonds, forming a three-dimensional network.

  13. A randomized, double-blind, placebo-controlled, proof-of-concept trial of creatine monohydrate as adjunctive treatment for bipolar depression.

    Science.gov (United States)

    Toniolo, Ricardo Alexandre; Silva, Michelle; Fernandes, Francy de Brito Ferreira; Amaral, José Antonio de Mello Siqueira; Dias, Rodrigo da Silva; Lafer, Beny

    2018-02-01

    Depressive episodes are a major cause of morbidity and dysfunction in individuals suffering from bipolar disorder. Currently available treatments for this condition have limited efficacy and new therapeutic options are needed. Extensive research in the pathophysiology of bipolar disorder points to the existence of mitochondrial and bioenergetic dysfunction. We hypothesized that creatine monohydrate, a nutraceutical that works as a mitochondrial modulator, would be effective as an adjunctive therapy for bipolar depression. We conducted a double-blind trial in which 35 patients with bipolar disorder type I or II in a depressive episode by DSM-IV criteria and in use of regular medication for the treatment of this phase of the disease were randomly allocated into two adjunctive treatment groups for 6 weeks: creatine monohydrate 6 g daily (N = 17) or placebo (N = 18). Primary efficacy was assessed by the change in the Montgomery-Åsberg Depression Rating Scale (MADRS). We did not find a statistically significant difference in the comparison between groups for the change in score on the MADRS after 6 weeks in an intention-to-treat (ITT) analysis (p = 0.560; Cohen's d = 0.231). However, we found significant superiority of creatine add-on vs. placebo when we considered the remission criterion of a MADRS score ≤ 12 at week 6 analyzing the outcome of the 35 randomized patients on ITT (52.9% remission in the creatine group vs. 11.1% remission in the placebo group) and of the 23 completers (66.7% remission in the creatine group vs. 18.2% remission in the placebo group) (p = 0.012; OR = 9.0 and p = 0.036; OR = 9.0, respectively). Two patients who received creatine switched to hypomania/mania early in the trial. No clinically relevant physical side-effects were reported or observed. This proof-of-concept study, aiming to restore brain bioenergetics using an adjunctive mitochondrial modulator, is not conclusive on the efficacy of creatine add-on for bipolar

  14. Creatine monohydrate supplementation does not increase muscle strength, lean body mass, or muscle phosphocreatine in patients with myotonic dystrophy type 1.

    Science.gov (United States)

    Tarnopolsky, Mark; Mahoney, Douglas; Thompson, Terry; Naylor, Heather; Doherty, Timothy J

    2004-01-01

    Creatine monohydrate (CrM) supplementation may increase strength in some types of muscular dystrophy. A recent study in myotonic muscular dystrophy type 1 (DM1) did not find a significant treatment effect, but measurements of muscle phosphocreatine (PCr) were not performed. We completed a randomized, double-blind, cross-over trial using 34 genetically confirmed adult DM1 patients without significant cognitive impairment. Participants received CrM (5 g, approximately 0.074 g/kg daily) and a placebo for each 4-month phase with a 6-week wash-out. Spirometry, manual muscle testing, quantitative isometric strength testing of handgrip, foot dorsiflexion, and knee extension, handgrip and foot dorsiflexion endurance, functional tasks, activity of daily living scales, body composition (total, bone, and fat-free mass), serum creatine kinase activity, serum creatinine concentration and clearance, and liver function tests were completed before and after each intervention, and muscle PCr/beta-adenosine triphosphate (ATP) ratios of the forearm flexor muscles were completed at the end of each phase. CrM supplementation did not increase any of the outcome measurements except for plasma creatinine concentration (but not creatinine clearance). Thus, CrM supplementation at 5 g daily does not have any effects on muscle strength, body composition, or activities of daily living in patients with DM1, perhaps because of a failure of the supplementation to increase muscle PCr/beta-ATP content.

  15. Quantifying low amorphous or crystalline amounts of alpha-lactose-monohydrate using X-ray powder diffraction, near-infrared spectroscopy, and differential scanning calorimetry.

    Science.gov (United States)

    Fix, I; Steffens, K J

    2004-05-01

    Efficient and accurate quantification of low amorphous and crystalline contents within pharmaceutical materials still remains a challenging task in the pharmaceutical industry. Since X-ray powder diffraction (XRPD) equipment has improved in recent years, our aim was 1) to investigate the possibility of substantially lowering the detection limits of amorphous or crystalline material to about 1% or 0.5% w/w respectively by applying conventional Bragg Brentano optics, combined with a fast and simple evaluation technique; 2) to perform these measurements within a short time to make it suitable for routine analysis; and 3) to subject the same data sets to a partial least squares regression (PLSR) in order to investigate whether it is possible to improve accuracy and precision compared to the standard integration method. Near-infrared spectroscopy (NIRS) and differential scanning calorimetry (DSC) were chosen as reference method. As model substance, alpha lactose monohydrate was chosen to create calibration curves based on predetermined mixtures of highly crystalline and amorphous substance. In contrast to DSC, XRPD and NIRS revealed an excellent linearity, precision, and accuracy with the percent of crystalline amount and a detectability down to about 0.5% w/w. Chemometric evaluation (partial least squares regression) applied to the XRPD data further improved the quality of our calibration.

  16. A comparative study of the influence of alpha-lactose monohydrate particle morphology on granule and tablet properties after roll compaction/dry granulation.

    Science.gov (United States)

    Grote, Simon; Kleinebudde, Peter

    2018-05-29

    The influence of particle morphology and size of alpha-lactose monohydrate on dry granules and tablets was studied. Four different morphologies were investigated: Two grades of primary crystals, which differed in their particle size and structure (compact crystals vs. agglomerates). The materials were roll compacted at different specific compaction forces and changes in the particle size distribution and the specific surface area were measured. Afterwards, two fractions of granules were pressed to tablets and the tensile strength was compared to that from tablets compressed from the raw materials. The specific surface area was increased induced by roll compaction/dry granulation for all materials. At increased specific compaction forces, the materials showed sufficient size enlargement. The morphology of lactose determined the strength of direct compressed tablets. In contrast, the strength of granule tablets was leveled by the previous compression step during roll compaction/dry granulation. Thus, the tensile strength of tablets compressed directly from the powder mixtures determined whether materials exhibited a loss in tabletability after roll compaction/dry granulation or not. The granule size had only a slight influence on the strength of produced tablets. In some cases, the fraction of smaller granules showed a higher tensile strength compared to the larger fraction.

  17. A comparative study on the effects of glucose monohydrate, hot water, and sodium pyrophosphate on quality parameters and microbial flora of deboned and matured brisket.

    Science.gov (United States)

    Gögüs, U; Bozoglu, F; Alpas, H

    2007-09-01

    Organic acids, hot water (HW), and chlorine have been commonly used in carcass decontamination for years. However, it has been observed that organic acids have adverse effects on color and are corrosive, while HW is discoloring. On the other hand, glucose fermentation by lactic acid bacteria in meat during the rigor period might be effective in microbial inhibition, without producing an adverse effect on the organoleptic quality of meat. Therefore, this study has aimed at finding an alternative meat decontamination procedure without any adverse effects. In this study, briskets were treated with 6 different applications: D (+) glucose monohydrate (GM) (16.51 g/100 mL, 15%) dip, HW dip, sodium pyrophosphate (SPP) and HW dip, GM + SPP + HW, and GM + HW combined dip. Then, the results of these applications were compared. First, GM + HW and GM + SPP + HW applications indicated more inhibition on Pseudomonas spp., Coliform and total Mesophile Aerob Bacteria growth, resulting in lower acidity loss (P < 0.01). Second, additional use of SPP with GM and HW did not enhance microbial inhibition (P < 0.01). Finally and most importantly, GM, 15%, improved a and b Hunter values significantly (P < 0.01), producing a very intense red meat color that can be very attractive for meat producers and consumers.

  18. Studies on the effect of different operational parameters on the crystallization kinetics of α-lactose monohydrate single crystals in aqueous solution

    Science.gov (United States)

    Parimaladevi, P.; Srinivasan, K.

    2014-09-01

    Supersaturation dependent nucleation, size and morphology of alpha-lactose monohydrate (α-LM) crystals from aqueous solution were investigated by adopting two different crystallization methods, slow evaporation and fast evaporation, in the supersaturation range between σ=0.05 and 1.30. The induction period of nucleation is comparatively long in case of slow evaporation and is very short in case of fast evaporation process as the interconversion between α-L and β-L is uncontrollable in the former and is under control in the latter case. Moreover α-LM crystals with tomahawk morphology were obtained throughout the supersaturation range by slow evaporation method whereas crystals with tomahawk, triangular and needle-like morphologies were obtained in supersaturation ranges σ=0.05-0.5, σ=0.5-0.9 and σ=0.9-1.30 respectively by fast evaporation method. Experimentally observed nucleation parameters were verified with theoretically deuced values. It is realized that the fast evaporation method employed in the present study is found to be highly efficient in controlling the interconversion between α-L and β-L as well as in suppressing the inhibitory activity of β molecule on the nucleation and growth of α-LM crystals when compared to conventional slow evaporation method and is successful in producing the industrially preferred needle-like crystals at high supersaturation ranges.

  19. Experimental and density functional theory (DFT): A dual approach to probe the key properties of creatininium L-tartrate monohydrate single crystal for nonlinear optical applications

    Science.gov (United States)

    Thirumurugan, R.; Babu, B.; Anitha, K.; Chandrasekaran, J.

    2017-12-01

    A novel organic nonlinear optical (NLO) material, creatininium L-tartrate monohydrate (CTM) was synthesized and it was grown as single crystals with optical quality. 1H and 13C NMR spectral studies were performed and molecular structure of synthesized CTM compound was confirmed. Single crystal X-ray diffraction (SXRD) analysis confirmed that CTM was crystallized in orthorhombic system with non-centrosymmetric (NCS), P212121, space group. The grown crystal exhibited admirable properties such as second harmonic generation efficiency (SHG) (1.9 times KDP), and high laser damage threshold (LDT) value of 3.7 GW cm-2. CTM crystal displayed high transparency (∼60%) in the visible and near-IR region with low cut-off wavelength at 249 nm. Photoluminescence study confirmed blue wavelength emission (∼463 nm) of grown crystal. Thermal and mechanical behaviours have been successfully analysed for grown crystals. The dielectric studies were carried out for grown crystal as a function of frequencies at different temperatures. Hirshfeld surface and fingerprint plots provided the percentage of individual interactions contributed by each atom. Moreover, density functional theory (DFT) calculations have been employed to probe the frontier molecular orbitals (FMOs) and first hyperpolarizability (β) analysis of the optimized CTM structure. These results validated CTM as a suitable NLO candidate and were discussed in this work.

  20. Creatine Monohydrate Enhances Energy Status and Reduces Glycolysis via Inhibition of AMPK Pathway in Pectoralis Major Muscle of Transport-Stressed Broilers.

    Science.gov (United States)

    Zhang, Lin; Wang, Xiaofei; Li, Jiaolong; Zhu, Xudong; Gao, Feng; Zhou, Guanghong

    2017-08-16

    Creatine monohydrate (CMH) contributes to reduce transport-induced muscle rapid glycolysis and improve meat quality of broilers, but the underlying mechanism is still unknown. Therefore, this study aimed to investigate the molecular mechanisms underlying the ameliorative effects of CMH on muscle glycolysis metabolism of transported broilers during summer. The results showed that 3 h transport during summer elevated chicken live weight loss and plasma corticosterone concentration; decreased muscle concentrations of ATP, creatine, and energy charge value; increased muscle AMP concentration and AMP/ATP ratio; and upregulated muscle mRNA expression of LKB1 and AMPKα2, as well as protein expression of p-LKB1 Thr189 and p-AMPKα Thr172 , which subsequently resulted in rapid glycolysis in the pectoralis major muscle and consequent reduction of meat quality. Dietary addition of CMH at 1200 mg/kg ameliorated transport-induced rapid muscle glycolysis and reduction of meat quality via enhancement of the energy-buffering capacity of intramuscular phosphocreatine/creatine system and inhibition of AMPK pathway.

  1. Evaluation of the repeated dose liver micronucleus assay using young adult rats with cyclophosphamide monohydrate: a report of a collaborative study by CSGMT/JEMS.MMS.

    Science.gov (United States)

    Matsumoto, Kazumi; Zaizen, Kazuyo; Miyamoto, Atsushi; Wako, Yumi; Kawasako, Kazufumi; Ishida, Hisao

    2015-03-01

    The repeated dose liver micronucleus (RDLMN) assay using young adult rats has the potential to detect liver carcinogens, and this assay could be integrated into general toxicological studies. In this study, in order to assess the performance of the assay, cyclophosphamide monohydrate (CP) was tested in a 14-day RDLMN assay. Based on the results of the 4-day repeated dose-finding study, 10 mg/kg/day of CP was selected as the highest dose and the lower doses were set at 5, 2.5, 1.25, and 0.625 mg/kg/day for the 14-day RDLMN assay. On the day after the completion of the dosing period, specimens of hepatocytes and bone marrow cells were prepared and the induction of micronuclei was assessed. No changes were observed in the incidences of micronucleated hepatocytes. Nevertheless, the incidences of micronucleated immature erythrocytes in the bone marrow were increased significantly at CP doses of 1.25 mg/kg/day or more. These findings are consistent with reports that CP induces tumors in various tissues but it does not induce liver tumors.

  2. Vibrational, DFT, and thermal analysis of 2,4,6-triamino-1,3,5-triazin-1-ium 3-(prop-2-enoyloxy) propanoate acrylic acid monosolvate monohydrate

    Science.gov (United States)

    Sangeetha, V.; Govindarajan, M.; Kanagathara, N.; Marchewka, M. K.; Drozd, M.; Anbalagan, G.

    2013-12-01

    New organic crystals of 2,4,6-triamino-1,3,5-triazin-1-ium 3-(prop-2-enoyloxy) propanoate acrylic acid monosolvate monohydrate (MAC) have been obtained from aqueous solution by the slow solvent evaporation method at room temperature. Single crystal X-ray diffraction analysis reveals that the compound crystallises in the triclinic system with centrosymmetric space group P-1. FT-IR and FT-Raman spectra of MAC have been recorded and analyzed. The molecular geometry and vibrational frequencies and intensity of the vibrational bands are interpreted with the aid of structure optimization based on density functional theory (DFT) B3LYP method with 6-31G(d,p) basis set. The results of the optimized molecular structure are presented and compared with the experimental X-ray diffraction data. The theoretical results show that the optimized geometry can well reproduce the crystal structure, and the calculated vibrational frequency values show good agreement with experimental values. A study of the electronic properties, such as HOMO and LUMO energies and Molecular electrostatic potential (MEP) were performed. Mulliken charges and NBO charges of the title molecule were also calculated and interpreted. Thermogravimetric analysis has been done to study the thermal behaviour of MAC. The 13C and 1H nuclear magnetic resonance (NMR) chemical shifts of the molecule are calculated by the gauge independent atomic orbital (GIAO) method and compared with experimental results.

  3. The role of hydrogen bonds in the crystals of 2-amino-4-methyl-5-nitropyridinium trifluoroacetate monohydrate and 4-hydroxybenzenesulfonate - X-ray and spectroscopic studies.

    Science.gov (United States)

    Bryndal, I; Marchewka, M; Wandas, M; Sąsiadek, W; Lorenc, J; Lis, T; Dymińska, L; Kucharska, E; Hanuza, J

    2014-04-05

    Two new organic-organic salts, 2-amino-4-methyl-5-nitropyridinium trifluoroacetate monohydrate (AMNP-TFA), and 2-amino-4-methyl-5-nitropyridinium 4-hydroxybenzenesulfonate (AMNP-HBS), were obtained and characterized by means of FT-IR, FT-Raman and single crystal X-ray crystallography. In the former crystal, the cations, anions and water molecules are linked into layers by three types of hydrogen bonds, NPH⋯O, NAH⋯O and OH⋯O. These layers are connected by weaker CH⋯O hydrogen bonds. In the latter crystal, the cations and anions form one-dimensional structure through a number of hydrogen-bonding interactions involving the OH, NH(+) and NH2 groups as donors. In this case the NPH⋯O and NAH⋯O hydrogen bonds are formed. The combination of interactions between cations and anions results in the formation of columns. Additionally, there are π-π stacking interactions between the columns. The obtained X-ray structural data are related to the vibrational spectra of the studied crystals. Copyright © 2013 Elsevier B.V. All rights reserved.

  4. Predictive factors of overall functioning improvement in patients with chronic schizophrenia and schizoaffective disorder treated with paliperidone palmitate and aripiprazole monohydrate.

    Science.gov (United States)

    Girardi, Paolo; Del Casale, Antonio; Rapinesi, Chiara; Kotzalidis, Georgios D; Splendori, Francesca; Verzura, Claudio; Trovini, Giada; Sorice, Serena; Carrus, Dario; Mancinelli, Iginia; Comparelli, Anna; De Filippis, Sergio; Francomano, Antonio; Ballerini, Andrea; Marcellusi, Andrea; Mennini, Francesco S; Ducci, Giuseppe; Sani, Gabriele; Pompili, Maurizio; Brugnoli, Roberto

    2018-05-01

    Long-acting injectable (LAI) antipsychotics can improve medication adherence and reduce hospitalisation rates compared with oral treatments. Paliperidone palmitate (PAL) and aripiprazole monohydrate (ARI) LAI treatments were associated with improvements in global functioning in patients with schizophrenia. The objective of this study was to assess the predictive factors of better overall functioning in patients with chronic schizophrenia and schizoaffective disorder treated with PAL and ARI. Enrolled were 143 (97 males, 46 females, mean age 38.24 years, SD = 12.65) patients with a diagnosis of schizophrenia or schizoaffective disorder, whom we allocated in two groups (PAL and ARI treatments). We assessed global functioning, amount of oral medications, adherence to oral treatment, and number of hospitalisations before LAI introduction and at assessment time point. Longer treatment time with LAIs (p schizoaffective disorder. Better improvement in functioning could be achieved with ARI in young individuals with recent illness onset and PAL in patients at risk for recurrent hospitalisations. Copyright © 2018 John Wiley & Sons, Ltd.

  5. Thermoelectrical and thermal analyses of copper(II) acetate monohydrate ZnO-matrix composite powder obtained by freeze-drying

    International Nuclear Information System (INIS)

    Bellini, Jusmar Valentin; Pineda, Edgardo Alfonso Gomez; Rocha, Raquel de Almeida; Ponzoni, Andre Luis de Lima; Paesano, Andrea

    2006-01-01

    The thermal history of freeze-dried mixtures of composite powders containing ZnO-matrix and (CH 3 COO) 2 Cu.H 2 O (copper(II) acetate monohydrate) was undertaken by thermal analysis (TA) coupled to thermoelectrical analysis (TEA). Experiments were carried out on compacted samples, under non-isothermal conditions, in air, up to 350 deg. C, by measuring the electrical resistance during heating, called thermoelectrical resistometry (TER), and by differential scanning calorimetry (DSC). Activation energy (E a ) for exothermal events related to the decomposition of (CH 3 COO) 2 Cu (copper(II) acetate, CuAc 2 ), observed within the range 225-325 deg. C, was estimated according to ASTM E 698 method. Values of E a equal to 154 and 155 kJ/mol were obtained by TER and DSC, respectively. TER showed that the thermal decomposition of CuAc 2 involves the liberation of electrons. Results also indicated that TER may be used as an alternative or complementary method for the study of the thermal decomposition mechanisms of transition metal(II) acetates

  6. [Antidotal effects of sulfhydryl compounds on acute poisonings by sodium ammonium dimethyl-2-(propane-1,3-dithiosulfate) monohydrate, nereistoxin and cartap].

    Science.gov (United States)

    Cao, B J; Chen, Z K; Chi, Z Q

    1990-03-01

    Sodium dimercaptopropanesulphonate (DMPS) and sodium dimercaptosuccinate (DMS) were discovered to be effective antidotes for acute poisoning of insecticides SCD [sodium ammonium dimethyl-2-(propane-1,3-dithiosulfate) monohydrate], nereistoxin (4-N,N-dimethylamino-1,2-dithiolane) and cartap (dihydronereistoxin dicarbamate). In mice, DMPS (250 mg/kg) or DMS (1000 mg/kg) ip 20 min before SCD increased LD50 of ig SCD from 97 to 374 or 251 mg/kg, respectively. The prophylactic effect of DMPS was better than that of DMS. Administration of DMPS prior to cartap increased LD50 of ig cartap from 130 to 375 mg/kg. The therapeutic effect of DMPS was also demonstrated in SCD-poisoned conscious rabbits. DMPS 62.5 mg/kg or DMS 500 mg/kg iv completely antagonized the neuromuscular blockade and respiratory depression caused by SCD, nereistoxin and cartap in anesthetized rabbits. The antagonism of SCD-induced neuromuscular blockade by cysteine (400 mg/kg, iv) was less effective and of shorter duration than that by DMPS and DMS. Dimercaprol 50 mg/kg im showed little effect on SCD-induced paralysis. The antagonistic actions of sulfhydryl compounds on neuromuscular blockade induced by these insecticides probably belong to chemical antagonism.

  7. Synthesis, optical, experimental and theoretical investigation of third order nonlinear optical properties of 8-hydroxyquinolinium 2-carboxy-6-nitrophthalate monohydrate single crystal

    Science.gov (United States)

    Bharathi, M. Divya; Bhuvaneswari, R.; Srividya, J.; Vinitha, G.; Prithiviraajan, R. N.; Anbalagan, G.

    2018-02-01

    Single crystals of 8-hydroxyquinolinium 2-carboxy-6-nitrophthalate monohydrate (8HQNP) were obtained from slow evaporation solution growth method using methanol-water (1:1) as a solvent. Powder X-ray diffraction was utilized to compute the unit cell parameters and dislocation density of 8HQNP crystal. The crystalline perfection of the as-grown crystal was investigated by high-resolution X-ray diffraction at room temperature. The molecular structure was analyzed by identifying the functional groups from FT-IR and FT-Raman spectra. The cut-off wavelength and the corresponding optical band gap obtained from an optical spectrum were 376 nm and 3.29 eV respectively. The dispersion nature of refractive index was investigated by the single-oscillator Wemple and Di-Domenico model. Red emission was observed in the photoluminescence spectrum when excited with 376 nm. The low birefringence and high laser damage threshold (8.538 GW/cm2) values dictate the suitability of the crystal for optical devices. Z-scan studies revealed the third order nonlinear absorption coefficient (β) and refractive index (n2) of the 8HQNP crystal. The theoretical value of third order nonlinear susceptibility obtained from density function theory is good accordance with the experimental value. The frontier molecular orbital energy gap decreases with increasing external electric field in different directions which attributed to the enhancement of the second hyperpolarizability. The grown title crystal is thermally stable up to 102 °C which was identified using thermal analysis. Mechanical strength of 8HQNP was estimated by using Vicker's microhardness studies.

  8. Studies on the concentration dependence of specific rotation of Alpha lactose monohydrate (α-LM) aqueous solutions and growth of α-LM single crystals

    Science.gov (United States)

    Vinodhini, K.; Divya Bharathi, R.; Srinivasan, K.

    2018-02-01

    Lactose is an optically active substance. As it is one of the reducing sugars, exhibits mutarotation in solution when it dissolves in any solvent. In solution, lactose exists in two isomeric forms, alpha-Lactose (α-L) and beta-lactose (β-L) through the mutarotation reaction. Mutarotation produces a dynamic equilibrium between two isomers in a solution and kinetics of this process determines the growth rate of alpha lactose monohydrate (α-LM) crystals. Since no data were available on the specific rotation of aqueous α-LM solutions at different concentrations at 33 °C, the initial experiments were carried out on the specific rotation of aqueous α-LM solutions at different concentrations at 33 °C. The specific rotations of the solutions were decreased with increasing time through the mutarotation reaction. The initial and final (equilibrium) specific rotations of the solutions were determined by using automatic digital polarimeter. The compositions of α and β-L in all prepared solutions were calculated from initial and final optical rotations by the method of Sharp and Doob. The composition of α-L decreased whereas, the composition of β-L increased in solutions with increasing concentration of α-LM at 33 °C. Experimental results revealed that this method could be easily and safely employed to study the dependence of specific rotation of solutions on their concentration. The effect of β-lactose on the morphology of nucleated α-LM single crystals has been studied at different experimental conditions.

  9. The study of the inhibitory effect of calcium oxalate monohydrate's crystallization by two medicinal and aromatic plants: Ammi visnaga and Punica granatum.

    Science.gov (United States)

    Kachkoul, R; Sqalli Houssaini, T; Miyah, Y; Mohim, M; El Habbani, R; Lahrichi, A

    2018-03-01

    Urinary lithiasis is a recurrent disease defined by the presence of calculi in the urinary tract. Most urinary calculi have as a major component calcium oxalate which occurs mainly in two crystalline forms: Calcium oxalate monohydrate (whewellite) and calcium oxalate dihydrate (weddellite). The target behind, this work is to study the inhibiting effect of the calcium oxalate's crystallization by the extract of the Ammi visnaga and the Punica granatum. The inhibition of crystallization has been studied in vitro with both the absence and the presence of the different concentrations of the extracts of the two plants. This study consists in measurement, with the UV-Visible spectrophotometer, the temporal evolution of the optical density at λ equal to 620nm corresponding to the formation of the crystals due to the mixing of metastable solutions of calcium and oxalate. The characterization of the crystals is carried out in parallel by both the Fourier transform infrared spectra (FT-IR) and the observation of the crystals with the help of an optical microscope. In this respect, the inhibition percentages were calculated from the turbidity slopes in the presence and absence of the extract. The results obtained were more effective, especially for Punica granatum with percentages of 97.8±0.12 and 83.46±1.34% against nucleation and aggregation, respectively, the order of Ammi visnaga was as follow: 73.25±0.81 and 59.44±3.3%. Thus, all correlation coefficients are greater than 0.95 and all coefficients of variation are less than 10%. The prevention and treatment of urinary lithiasis and especially in the case of recurrence by plants remains an alternative choice for medical methods. This study justified the efficacy of the plants Ammi visnaga and in particular Punica granatum against the crystallization of calcium oxalate. 3. Copyright © 2017 Elsevier Masson SAS. All rights reserved.

  10. Effects of creatine monohydrate supplementation on exercise-induced apoptosis in athletes: A randomized, double-blind, and placebo-controlled study

    Directory of Open Access Journals (Sweden)

    Rahman Rahimi

    2015-01-01

    Full Text Available Background: Creatine monohydrate (CrM has been shown to be beneficial to health due to its antioxidant potential. Strenuous exercise is associated with oxidative stress, which could lead to apoptosis. We investigated the ability of CrM in amelioration of apoptosis induced by incremental aerobic exercise (AE to exhaustion in young athletes. Materials and Methods: In a placebo-controlled, double-blind, randomized, parallel study, 31 young athletes (age 19.52 ± 2.75 years, body mass 79.24 ± 16.13 kg, height 1.73 ± 6.49 m, body fat 16.37% ± 5.92% were randomly assigned to CrM (4 × 5 g/day, n = 15 or placebo (PL: 4 × 5 g/day of maltodextrine powder; n = 16 to investigate the effect of 7 days CrM on serum p53 and insulin-like growth factor-1 (IGF-1 concentration after acute incremental AE test to exhaustion. Subjects performed AE before (test 1 and after 7 days of supplementation (test 2. Results: Before supplementation, AE to exhaustion induced a significant increase in serum p53 and IGF-1 concentrations at both CrM and PL groups (P 0.05. Conclusion: Our results suggest that supplementation with CrM prevents apoptosis, as measured by decreases in p53 concentration, induced by AE to exhaustion in young athletes. However, CrM had no effect on IGF-1 concentration after AE to exhaustion in young athletes.

  11. A buffered form of creatine does not promote greater changes in muscle creatine content, body composition, or training adaptations than creatine monohydrate

    Directory of Open Access Journals (Sweden)

    Jagim Andrew R

    2012-09-01

    Full Text Available Abstract Background Creatine monohydrate (CrM has been consistently reported to increase muscle creatine content and improve high-intensity exercise capacity. However, a number of different forms of creatine have been purported to be more efficacious than CrM. The purpose of this study was to determine if a buffered creatine monohydrate (KA that has been purported to promote greater creatine retention and training adaptations with fewer side effects at lower doses is more efficacious than CrM supplementation in resistance-trained individuals. Methods In a double-blind manner, 36 resistance-trained participants (20.2 ± 2 years, 181 ± 7 cm, 82.1 ± 12 kg, and 14.7 ± 5% body fat were randomly assigned to supplement their diet with CrM (Creapure® AlzChem AG, Trostberg, Germany at normal loading (4 x 5 g/d for 7-days and maintenance (5 g/d for 21-days doses; KA (Kre-Alkalyn®, All American Pharmaceutical, Billings, MT, USA at manufacturer’s recommended doses (KA-L, 1.5 g/d for 28-days; or, KA with equivalent loading (4 x 5 g/d for 7-days and maintenance (5 g/d doses of CrM (KA-H. Participants were asked to maintain their current training programs and record all workouts. Muscle biopsies from the vastus lateralis, fasting blood samples, body weight, DEXA determined body composition, and Wingate Anaerobic Capacity (WAC tests were performed at 0, 7, and 28-days while 1RM strength tests were performed at 0 and 28-days. Data were analyzed by a repeated measures multivariate analysis of variance (MANOVA and are presented as mean ± SD changes from baseline after 7 and 28-days, respectively. Results Muscle free creatine content obtained in a subgroup of 25 participants increased in all groups over time (1.4 ± 20.7 and 11.9 ± 24.0 mmol/kg DW, p = 0.03 after 7 and 28-days, respectively, with no significant differences among groups (KA-L −7.9 ± 22.3, 4.7 ± 27.0; KA-H 1.0 ± 12.8, 9.1

  12. A buffered form of creatine does not promote greater changes in muscle creatine content, body composition, or training adaptations than creatine monohydrate.

    Science.gov (United States)

    Jagim, Andrew R; Oliver, Jonathan M; Sanchez, Adam; Galvan, Elfego; Fluckey, James; Riechman, Steven; Greenwood, Michael; Kelly, Katherine; Meininger, Cynthia; Rasmussen, Christopher; Kreider, Richard B

    2012-09-13

    Creatine monohydrate (CrM) has been consistently reported to increase muscle creatine content and improve high-intensity exercise capacity. However, a number of different forms of creatine have been purported to be more efficacious than CrM. The purpose of this study was to determine if a buffered creatine monohydrate (KA) that has been purported to promote greater creatine retention and training adaptations with fewer side effects at lower doses is more efficacious than CrM supplementation in resistance-trained individuals. In a double-blind manner, 36 resistance-trained participants (20.2 ± 2 years, 181 ± 7 cm, 82.1 ± 12 kg, and 14.7 ± 5% body fat) were randomly assigned to supplement their diet with CrM (Creapure® AlzChem AG, Trostberg, Germany) at normal loading (4 x 5 g/d for 7-days) and maintenance (5 g/d for 21-days) doses; KA (Kre-Alkalyn®, All American Pharmaceutical, Billings, MT, USA) at manufacturer's recommended doses (KA-L, 1.5 g/d for 28-days); or, KA with equivalent loading (4 x 5 g/d for 7-days) and maintenance (5 g/d) doses of CrM (KA-H). Participants were asked to maintain their current training programs and record all workouts. Muscle biopsies from the vastus lateralis, fasting blood samples, body weight, DEXA determined body composition, and Wingate Anaerobic Capacity (WAC) tests were performed at 0, 7, and 28-days while 1RM strength tests were performed at 0 and 28-days. Data were analyzed by a repeated measures multivariate analysis of variance (MANOVA) and are presented as mean ± SD changes from baseline after 7 and 28-days, respectively. Muscle free creatine content obtained in a subgroup of 25 participants increased in all groups over time (1.4 ± 20.7 and 11.9 ± 24.0 mmol/kg DW, p = 0.03) after 7 and 28-days, respectively, with no significant differences among groups (KA-L -7.9 ± 22.3, 4.7 ± 27.0; KA-H 1.0 ± 12.8, 9.1 ± 23.2; CrM 11.3 ± 23.9, 22.3 ± 21

  13. An Open-Label Pilot Study of Combined Augmentation With Creatine Monohydrate and 5-Hydroxytryptophan for Selective Serotonin Reuptake Inhibitor- or Serotonin-Norepinephrine Reuptake Inhibitor-Resistant Depression in Adult Women.

    Science.gov (United States)

    Kious, Brent M; Sabic, Hana; Sung, Young-Hoon; Kondo, Douglas G; Renshaw, Perry

    2017-10-01

    Many women with major depressive disorder (MDD) respond inadequately to standard treatments. Augmentation of conventional antidepressants with creatine monohydrate and 5-hydroxytryptophan (5-HTP) could correct deficits in serotonin production and brain bioenergetics associated with depression in women, yielding synergistic benefit. We describe an open-label study of 5-HTP and creatine augmentation in women with MDD who had failed selective serotonin reuptake inhibitor (SSRI) or serotonin-norepinephrine reuptake inhibitor (SNRI) monotherapy. Fifteen women who were adequately adherent to an SSRI or SNRI and currently experiencing MDD, with a 17-item Hamilton Depression Rating Scale (HAM-D) score of 16 or higher, were treated with 5 g of creatine monohydrate daily and 100 mg of 5-HTP twice daily for 8 weeks, with 4 weeks of posttreatment follow-up. The primary outcome was change in mean HAM-D scores. Mean HAM-D scores declined from 18.9 (SD, 2.5) at pretreatment visits to 7.5 (SD, 4.4) (P creatine and 5-HTP may represent an effective augmentation strategy for women with SSRI- or SNRI-resistant depression. Given the limitations of this small, open-label trial, future study in randomized, placebo-controlled trials is warranted.

  14. Treatment with Creatine Monohydrate in Spinal and Bulbar Muscular Atrophy: Protocol for a Randomized, Double-Blind, Placebo-Controlled Trial.

    Science.gov (United States)

    Hijikata, Yasuhiro; Katsuno, Masahisa; Suzuki, Keisuke; Hashizume, Atsushi; Araki, Amane; Yamada, Shinichiro; Inagaki, Tomonori; Ito, Daisuke; Hirakawa, Akihiro; Kinoshita, Fumie; Gosho, Masahiko; Sobue, Gen

    2018-03-05

    Although spinal and bulbar muscular atrophy (SBMA) has been classified as a motor neuron disease, several reports have indicated the primary involvement of skeletal muscle in the pathogenesis of this devastating disease. Recent studies reported decreased intramuscular creatine levels in skeletal muscles in both patients with SBMA and transgenic mouse models of SBMA, which appears to contribute to muscle weakness. The present study aimed to examine the efficacy and safety of oral creatine supplementation to improve motor function in patients with SBMA. A randomized, double-blind, placebo-controlled, three-armed clinical trial was conducted to assess the safety and efficacy of creatine therapy in patients with SBMA. Patients with SBMA eligible for this study were assigned randomly in a 1:1:1 ratio to each group of placebo, 10 g, or 15 g daily dose of creatine monohydrate in a double-blind fashion. Participants took creatine or placebo orally 3 times a day for 8 weeks. Outcome measurements were results of neurological assessments, examinations, and questionnaires collected at baseline and at weeks 4, 8, and 16 after a washout period. The primary endpoint was the change in handgrip strength values from baseline to week 8. The secondary endpoints included the following: results of maximum voluntary isometric contraction tests of extremities; tongue pressure; results of the 15-foot timed walk test and the rise from bed test; modified quantitative myasthenia gravis score; respiratory function test results; activities of daily living assessed with the Revised Amyotrophic Lateral Sclerosis Functional Rating Scale and the Spinal and Bulbar Muscular Atrophy Functional Rating Scale; skeletal muscle mass measured with dual-energy X-ray absorptiometry; urinary 8-hydroxydeoxyguanosine levels; and questionnaires examining the quality of life, swallowing function, and fatigue. Participant enrollment in the trial started from June 2014 and follow-up was completed in July 2015. The

  15. EPR study of gamma irradiated N-methyl taurine (C 3H 9NO 3S) and sodium hydrogen sulphate monohydrate (NaHSO 3·H 2O) single crystals

    Science.gov (United States)

    Yıldırım, İlkay; Karabulut, Bünyamin

    2011-03-01

    EPR study of gamma irradiated C 3H 9NO 3S and NaHSO 3.H 2O single crystals have been carried out at room temperature. There is one site for the radicals in C 3H 9NO 3S and two magnetically distinct sites for the radicals in NaHSO 3. The observed lines in the EPR spectra have been attributed to the species of SO3- and RH radicals for N-methyl taurine, and to the SO3- and OH radicals for sodium hydrogen sulfate monohydrate single crystals. The principal values of the g for SO3-, the hyperfine values of RH and OH proton splitting have been calculated and discussed.

  16. 4-Methoxybenzamidinium hydrogen oxalate monohydrate

    Directory of Open Access Journals (Sweden)

    Simona Irrera

    2012-12-01

    Full Text Available The title hydrated salt, C8H11N2O+·C2HO4−·H2O, was synthesized by a reaction of 4-methoxybenzamidine (4-amidinoanisole and oxalic acid in water solution. In the cation, the amidinium group forms a dihedral angle of 15.60 (6° with the mean plane of the benzene ring. In the crystal, each amidinium unit is bound to three acetate anions and one water molecule by six distinct N—H...O hydrogen bonds. The ion pairs of the asymmetric unit are joined by two N—H...O hydrogen bonds into ionic dimers in which the carbonyl O atom of the semi-oxalate anion acts as a bifurcated acceptor, thus generating an R12(6 motif. These subunits are then joined through the remaining N—H...O hydrogen bonds to adjacent semi-oxalate anions into linear tetrameric chains running approximately along the b axis. The structure is stabilized by N—H...O and O—H...O intermolecular hydrogen bonds. The water molecule plays an important role in the cohesion and the stability of the crystal structure being involved in three hydrogen bonds connecting two semi-oxalate anions as donor and a benzamidinium cation as acceptor.

  17. 1-Azaniumylcyclobutane-1-carboxylate monohydrate

    Directory of Open Access Journals (Sweden)

    Ray J. Butcher

    2014-02-01

    Full Text Available In the title compound, C5H9NO2·H2O, the amino acid is in the usual zwitterionic form involving the α-carboxylate group. The cyclobutane backbone of the amino acid is disordered over two conformations, with occupancies of 0.882 (7 and 0.118 (7. In the crystal, N—H...O and O—H...O hydrogen bonds link the zwitterions [with the water molecule involved as both acceptor (with the NH3+ and donor (through a single carboxylate O from two different aminocyclobutane carboxylate moities], resulting in a two-dimensional layered structure lying parallel to (100.

  18. Synthesis and crystal structure of a new 2,6-dimethyl piperazine-1,4-diium perchlorate monohydrate: [C{sub 6}H{sub 16}N{sub 2}](ClO{sub 4}){sub 2} · H{sub 2}O

    Energy Technology Data Exchange (ETDEWEB)

    Mleh, C. Ben [Université de Carthage, Laboratoire de Chimie des Matériaux, Faculté des Sciences de Bizerte (Tunisia); Roisnel, T. [Université de Rennes I, Centre de Diffractométrie X, UMR 6226 CNRS, Unité Sciences Chimiques de Rennes (France); Marouani, H., E-mail: houda.marouani@fsb.rnu.tn [Université de Carthage, Laboratoire de Chimie des Matériaux, Faculté des Sciences de Bizerte (Tunisia)

    2017-03-15

    A proton transfer compound 2,6-dimethyl piperazine-1,4-diium perchlorate monohydrate was synthesized by slow evaporation at room temperature using 2,6-dimethyl piperazine as template. The asymmetric unit contains one organic dication, two crystal graphically independent perchlorate anions and one water molecule. Each organic entities is engaged in a large number of bifurcated and non-bifurcated N–H···O (O) and C–H···O hydrogen bonds with different species and enhanced the three dimensional supramolecular network. In addition, the diprotonated piperazine ring adopts a chair conformation with the methyl groups occupying equatorial positions.

  19. Stone clearance after extracorporeal shockwave lithotripsy in patients with solitary pure calcium oxalate stones smaller than 1.0 cm in the proximal ureter, with special reference to monohydrate and dihydrate content.

    Science.gov (United States)

    Ichiyanagi, Osamu; Nagaoka, Akira; Izumi, Takuji; Kawamura, Yuko; Tsukigi, Masaaki; Ishii, Tatsuya; Ohji, Hiroshi; Kato, Tomoyuki; Tomita, Yoshihiko

    2013-04-01

    The aim of this study was to assess stone-free rates following extracorporeal shockwave lithotripsy (ESWL) of pure calcium oxalate (CaOx) stones in the proximal ureter. The investigators retrospectively examined 53 patients with 5-10 mm pure CaOx stones in the proximal ureter from the medical archives of 593 consecutive patients treated with ESWL. The compositions of calcium oxalate monohydrate (COM) and dihydrate (COD) in a given stone were determined by infrared spectrometry. Stone size, attenuation number and stone-to-skin distance (SSD) were measured using plain radiography and computed tomography (CT). ESWL success was evaluated by stone-free status after the first single session. On average, calculi were 8.0 × 5.3 mm in size, with an SSD of 11.0 cm. The mean CT attenuation value was 740.1 HU. Attenuation numbers correlated significantly with stone diameter (r = 0.49), but had no correlation with the stone content of COM or COD. A negative correlation was observed between COM and COD content (r = -0.925). With regard to patients' physical characteristics and COM and COD content, no differences were found between study subgroups with stone-free and residual status (n = 38 and 15, respectively). There were also no differences in clinical features between patient subgroups with COM- or COD-predominant stones (n = 22 and 31, respectively). The findings indicated that the differences in COM and COD content of CaOx stones had no impact on stone clearance after ESWL and that a favorable stone-free rate of the stones treated with ESWL may be achieved independently of CaOx hydration.

  20. L-leucine, beta-hydroxy-beta-methylbutyric acid (HMB) and creatine monohydrate prevent myostatin-induced Akirin-1/Mighty mRNA down-regulation and myotube atrophy.

    Science.gov (United States)

    Mobley, Christopher Brooks; Fox, Carlton D; Ferguson, Brian S; Amin, Rajesh H; Dalbo, Vincent J; Baier, Shawn; Rathmacher, John A; Wilson, Jacob M; Roberts, Michael D

    2014-01-01

    The purpose of this study was to examine if L-leucine (Leu), β-hydroxy-β-methylbutyrate (HMB), or creatine monohydrate (Crea) prevented potential atrophic effects of myostatin (MSTN) on differentiated C2C12 myotubes. After four days of differentiation, myotubes were treated with MSTN (10 ng/ml) for two additional days and four treatment groups were studied: 1) 3x per day 10 mM Leu, 2) 3x per day 10 mM HMB, 3) 3x per day 10 mM Crea, 4) DM only. Myotubes treated with DM without MSTN were analyzed as the control condition (DM/CTL). Following treatment, cells were analyzed for total protein, DNA content, RNA content, muscle protein synthesis (MPS, SUnSET method), and fiber diameter. Separate batch treatments were analyzed for mRNA expression patterns of myostatin-related genes (Akirin-1/Mighty, Notch-1, Ski, MyoD) as well as atrogenes (MuRF-1, and MAFbx/Atrogin-1). MSTN decreased fiber diameter approximately 30% compared to DM/CTL myotubes (p HMB and Crea prevented MSTN-induced atrophy. MSTN did not decrease MPS levels compared to DM/CTL myotubes, but MSTN treatment decreased the mRNA expression of Akirin-1/Mighty by 27% (p HMB myotubes had similar Akirin-1/Mighty and MyoD mRNA levels compared to DM/CTL myotubes. Furthermore, MSTN + Crea myotubes exhibited a 36% (p HMB and Crea may reduce MSTN-induced muscle fiber atrophy by influencing Akirin-1/Mighty mRNA expression patterns. Future studies are needed to examine if Leu, HMB and Crea independently or synergistically affect Akirin-1/Mighty expression, and how Akirin-1/Mighty expression mechanistically relates to skeletal muscle hypertrophy in vivo.

  1. Transplacental passage of Pt after treatment with the new triamine complex cis-diaminechloro-[2-(diethylamino) ethyl 4-amino-benzoate, N{sup 4}]-chloride platinum (II) monohydrochloride monohydrate

    Energy Technology Data Exchange (ETDEWEB)

    Ognio, Emanuela; Lapide, Maddalena [Servizio Modelli Animali, Istituto Nazionale per la Ricerca sul Cancro, Genova (Italy); Chiavarina, Barbara; Viale, Maurizio [U.O. Farmacologia e Neuroscienze, Lab. Farmacologia Tossicologica, Istituto Nazionale per la Ricerca sul Cancro, Lgo R. Benzi, 10, Genova (Italy); Caviglioli, Gabriele [Universita di Genova, Dipartimento di Chimica e Tecnologie Farmaceutiche e Alimentari, Genova (Italy)

    2004-10-01

    Cis-diaminechloro-[2-(diethylamino) ethyl 4-amino-benzoate, N{sup 4}]-chloride platinum (II) monohydrochloride monohydrate (DPR) is a monofunctional Pt triamine complex synthesized starting from cisplatin and procaine hydrochloride, characterized by a good antitumor activity coupled with low toxic effects and able to impair prenatal development of mice but at doses outside or just in the upper range of therapeutic doses. In the present paper the transplacental passage of DPR-derived Pt was investigated in CD1 mice on days 9, 13, 16 and 18 of pregnancy, 24 h after ip administration of 21 mg/kg DPR. For comparison, groups of mice were treated with an equivalent Pt-containing dose of cisplatin (10.7 mg/kg). Similarly to cisplatin, small amounts of Pt were detected in fetuses on day 9. From day 13 of gestation the concentration of DPR- and cisplatin-derived Pt increased up to the highest fetal concentrations detected on day 16. On day 18 the concentration of Pt decreased. Most importantly, on days 13-18 of pregnancy cisplatin-derived Pt was always significantly higher than that assayed after DPR administration. In addition, on day 13 of pregnancy Pt exposure of fetuses was significantly higher when dams were treated with cisplatin (AUC{sub 0.5-24}= 3.40 vs. 4.95 {mu}g.h/g). Finally, it is worth noting that serum decay of Pt after DPR or cisplatin administration in adult female mice was similar with AUC{sub 0.13-2h} s of 7.5 and 6.6 {mu}g.h/ml, respectively. When we determined the concentration of Pt into the main organs of fetuses from dams treated with either DPR or cisplatin on day 18 of gestation, we observed a different organ distribution. In fact, while the concentration of DPR-derived Pt was greater in the heart (1.08{+-}0.30 vs. 0.78{+-}0.35 {mu}g/g, p<0.10), an opposite situation was found in the kidney (0.51{+-}0.20 vs. 0.69{+-}0.22 {mu}g/g, p<0.05). In conclusion, our data show that DPR may pass through the placenta with an efficiency significantly lower than

  2. A new copper(II) chelate complex with tridentate ligand: Synthesis, crystal and molecular electronic structure of aqua-(diethylenetriamine-N, N‧, N‧‧)-copper(II) sulfate monohydrate and its fire retardant properties

    Science.gov (United States)

    Lavrenyuk, H.; Mykhalichko, O.; Zarychta, B.; Olijnyk, V.; Mykhalichko, B.

    2015-09-01

    The crystals of a new aqua-(diethylenetriamine-N, N‧, N‧‧)-copper(II) sulfate monohydrate have been synthesized by direct interaction of solid copper(II) sulfate pentahydrate with diethylenetriamine (deta). The crystal structure of [Cu(deta)H2O]SO4ṡH2O (1) has been determined by X-ray diffraction methods at 100 K and characterized using X-ray powder diffraction pattern: space group P 1 bar, a = 7.2819(4), b = 8.4669(4), c = 8.7020(3) Å, α = 83.590(3), β = 89.620(4), γ = 84.946(4)°, Z = 2. The environment of the Cu(II) atom is a distorted, elongated square pyramid which consists of three nitrogen atoms of the deta molecule and oxygen atom of the water molecule in the basal plane of the square pyramid (the average lengths of the in-plane Cu-N and Cu-O bonds are 2.00 Å). The apical position of the coordination polyhedron is occupied by complementary oxygen atom of the sulfate anion (the length of the axial Cu-O bond is 2.421(1) Å). The crystal packing is governed by strong hydrogen bonds of O-H⋯O and N-H⋯O types. The ab initio quantum-chemical calculations have been performed by the restricted Hartree-Fock method with a basis set 6-31∗G using the structural data of [Cu(deta)H2O]SO4ṡH2O. It has been ascertained that the degenerate d-orbitals of the Cu2+ ion split under the co-action of both the square-pyramidal coordination and the chelation. It is significant that visually observed crystals color (blue-violet) of the [Cu(deta)H2O]SO4ṡH2O complex is in good agreement with the calculated value of wavelength of visible light (λ = 5735 Å) which is closely related to the energy of the absorbed photon (Δ = 2.161 eV). Furthermore, the stereo-chemical aspect of influence of the CuSO4 upon combustibility of modified epoxy-amine polymers has been scrutinized.

  3. Effects of (-)-S-2,8-dimethyl-3-methylene-1-oxa-8-azaspiro[4,5]decane L-tartrate monohydrate (YM796), a novel muscarinic agonist, on disturbance of passive avoidance learning behavior in drug-treated and senescence-accelerated mice.

    Science.gov (United States)

    Suzuki, M; Yamaguchi, T; Ozawa, Y; Ohyama, M; Yamamoto, M

    1995-11-01

    Effects of YM796 (-)-S-2,8-dimethyl-3-methylene-1-oxa-8-azaspiro[4,5]decane L-tartrate monohydrate; a novel muscarinic agonist, were observed on disturbance of passive avoidance learning behavior in drug- (protein synthesis inhibitor and anticholinergic drugs) treated and senescence-accelerated mice in comparison with those of a muscarinic agonist (AF102B) and acetylcholinesterase inhibitors (E2020 (1-benzyl-4-[(5,6-dimethoxy-1-indanone-2-yl) methyl] piperidene hydrochloride), NIK247 [9-amino-2,3,5,6,7,8-hexahydro-1H-cyclopenta(b)-quinoline monohydrate hydrochloride], THA (9-amino-1,2,3,4-tetrahydroacridine) and physostigmine). All tested drugs administered before training significantly prolonged the shortened latency of step-through induced by the protein synthesis inhibitor cycloheximide (150 mg/kg s.c.). This shortened latency was also significantly prolonged when YM796 was administered immediately after training, but not when administered before the test trial. The ameliorating effect of YM796 on the impairment in learning behavior by cycloheximide was significantly suppressed by pirenzepine (0.1 micrograms/mouse i.c.v.). When administered before training, all test drugs prolonged the shortened latency of step-through induced by treatment with the anticholinergic drugs [scopolamine (1 mg/kg s.c.) and hemicholinium-3 (0.3 microgram/mouse i.c.v.)], suggesting that they ameliorated the impairment of learning behavior. This shortened latency in scopolamine-treated mice was also significantly prolonged by YM796, AF102B, E2020, NIK247 and physostigmine when administered immediately after training, but not when administered before the test trial. The pharmacological actions of YM796 administered immediately after training and before the test trial in hemicholinium-3-treated mice were similar to those in scopolamine-treated mice.(ABSTRACT TRUNCATED AT 250 WORDS)

  4. Efeitos da suplementação prolongada de creatina mono-hidratada sobre o desempenho anaeróbio de adultos jovens treinados Effects of long-term creatine monohydrate supplementation on anaerobic performance of trained young adults

    Directory of Open Access Journals (Sweden)

    Leandro Ricardo Altimari

    2010-06-01

    Full Text Available O objetivo do presente estudo foi investigar o impacto de oito semanas de suplementação de creatina mono-hidratada (Crm sobre o desempenho anaeróbio de adultos jovens treinados. Vinte e seis estudantes de educação física, do sexo masculino, saudáveis, foram divididos aleatoriamente em grupo creatina (GCr, n = 13; 22,5 ± 2,7 anos; 74,9 ± 6,8kg, 178,5 ± 4,8cm e grupo placebo (GPl, n = 13; 22,9 ± 3,2 anos, 71,9 ± 11,3kg, 178,6 ± 4,0cm. Os indivíduos ingeriram em sistema duplo-cego doses de Crm ou placebo-maltodextrina (20 g.d-1 por 5 dias e 3 g.d-1 por 51 dias subsequentes. Ambos os grupos tiveram seus hábitos alimentares e os níveis de aptidão física controlados anteriormente. O teste anaeróbio de Wingate (TW foi usado para avaliar o desempenho anaeróbio antes e após o período de ingestão de Crm ou placebo. Os índices de desempenho analisados foram: potência pico relativa (PPR, potência média relativa (PMR, trabalho total relativo (TTR e índice de fadiga (IF. Para tratamento estatístico foi utilizado ANOVA, seguido pelo teste de post hoc Tukey, quando PThe objective of the present study was to investigate the impact of eight weeks of creatine monohydrate (Crm supplementation on the anaerobic performance of young trained adults. Twenty-six healthy male physical education students were randomly divided in creatine group (CrG, n = 13; 22.5 ± 2.7 years; 74.9 ± 6.8 kg; 178.5 ± 4.8 cm and placebo group (PlG, n = 13; 22.9 ± 3.2 years; 71.9 ± 11.3 kg; 178.6 ± 4.0 cm. The subjects received in a double-blind system a Crm or placebo-maltodextrin dose (20 g.d-1 for 5 days and 3 g.d-1 for 51 subsequent days. Both groups had their eating habits and levels of physical fitness previously controlled. The Wingate anaerobic test (WT was used to evaluate the anaerobic performance before and after the ingestion period of Crm or placebo. The performance indexes assessed were: relative peak power (RPP, relative mean power (RMP

  5. 3-Carboxyquinolin-1-ium-2-carboxylate monohydrate

    Directory of Open Access Journals (Sweden)

    Qing Zhang

    2012-03-01

    Full Text Available The title compound, C11H7NO4·H2O, contains a 3-carboxyquinolin-1-ium-2-carboxylate (qda zwitterion and one water molecule. In the crystal, pairs of N—H...O hydrogen bonds link the molecules into inversion dimers, and these dimers are further connected by O—H...O hydrogen bonds into a three-dimensional supramolecular architecture. In addition, π–π interactions occur between pyridine and benzene rings from different qda ligands [centroid–centroid distance = 3.749 (1 Å] and the dihedral angles of the –CO2H and –CO2 groups to the quinoline system are 8.47 (3 and 88.16 (6°, respectively.

  6. The acidic phosphite of lanthanum monohydrate

    International Nuclear Information System (INIS)

    Tijani, N.; Durand, J.; Cot, L.

    1988-01-01

    La(HPO 3 H) 3 .H 2 O, M r =399.81, triclinic, Panti 1, a=8.054 (2), b=9.672 (3), c=7.224 (2) A, V=458.15 A 3 , α=111.35 (2), β=75.77 (2), γ=118.66 (2) 0 , Z=2, D m =2.88 (1), D x =2.906 Mg m -3 , λ(MoKα)=0.71069 A, μ(MoKα)=7.14 mm -1 , F(000)=380, T=293 K, R=0.038 for 868 independent reflexions. The structure consists of three phosphite anions connected by a strong hydrogen bond. The La 3+ cation is coordinated by seven O atoms of phosphite anions and one O atom of the water molecule. (orig.)

  7. Tris(2-carbamoylguanidinium) hydrogen fluorophosphonate fluorophosphonate monohydrate

    Czech Academy of Sciences Publication Activity Database

    Fábry, Jan; Fridrichová, M.; Dušek, Michal; Fejfarová, Karla; Krupková, Radmila

    2012-01-01

    Roč. 68, č. 20 (2012), o47-048 ISSN 1600-5368 R&D Projects: GA ČR GA203/09/0878 Grant - others:AV ČR(CZ) AP0701 Program:Akademická prémie - Praemium Academiae Institutional research plan: CEZ:AV0Z10100521 Keywords : structure analysis * hydrogen bond pattern * triocofluorophosphates Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.347, year: 2011

  8. Potassium tetracyanidoaurate(III monohydrate: a redetermination

    Directory of Open Access Journals (Sweden)

    Nobuyuki Matsushita

    2017-03-01

    Full Text Available The structure of the title metal complex salt, K[Au(CN4]·H2O, has been redetermined using X-ray diffraction data at 173 K in order to improve the precision. The previous determination was based on neutron diffraction data [Bertinotti & Bertinotti (1970. Acta Cryst. B26, 422–428]. The title compound crystallizes in the space group P212121 with one potassium cation, one [Au(CN4]− anion and one water molecule in the asymmetric unit. The AuIII atom lies on a general position and has an almost square-planar coordination sphere defined by four cyanide ligands. Interactions between the potassium cation and N atoms of the complex anion, as well as O—H...N hydrogen bonds, lead to the formation of a three-dimensional framework structure.

  9. N′-(3-Bromo-4-methoxybenzylidenenicotinohydrazide monohydrate

    Directory of Open Access Journals (Sweden)

    Feng-Yu Bao

    2009-09-01

    Full Text Available In the title compound, C14H12BrN3O2·H2O, the benzene ring is oriented at a dihedral angle of 39.66 (11° with respect to the pyridine ring. The solvent water molecule links with the organic compound via O—H...O, O—H...N and N—H...O hydrogen bonding.

  10. Piperazin-1-ium 4-aminobenzoate monohydrate

    Directory of Open Access Journals (Sweden)

    P. Sivakumar

    2016-05-01

    Full Text Available The asymmetric unit of the title hydrated salt, C4H11N2+·C7H6NO2−·H2O, contains a piperazin-1-ium cation, a 4-aminobenzoate anion and a water molecule. One NH group of the piperazine ring is protonated and this ring adopts a chair conformation. The anion of this salt is generated by deprotonation of the OH group of the carboxylic acid substituent of 4-aminobenzoic acid. The benzene ring makes a dihedral angle of 2.6 (2° with the carboxylate substituent. The anion and the solvent water molecule are linked by an N—H...O hydrogen bond. Additional N—H...O and O—H...O hydrogen bonds connect adjacent anions through the water molecules, generating a two-dimensional network parallel to (100, forming R33(12 ring motifs. Adjacent cations are linked by N—H...N hydrogen bonds into infinite chains along (001. These chains are linked to the two-dimensional network of anions and water molecules by another N—H...O hydrogen bond, forming a three-dimensional network.

  11. N-(2,5-Dimethylphenylsuccinamic acid monohydrate

    Directory of Open Access Journals (Sweden)

    B. S. Saraswathi

    2011-08-01

    Full Text Available In the title compound, C12H15NO3·H2O, the conformation of the N—H bond in the amide segment is syn to the ortho-methyl group and anti to the meta-methyl group in the benzene ring. Further, the conformations of the amide O and the carbonyl O atom of the acid segment are anti to the adjacent methylene H atoms. The C=O and O—H bonds of the acid group are syn to one another. The structure shows an interesting hydrogen-bonding pattern with the water molecule forming hydrogen bonds with three different molecules of the compound. In the crystal, molecules are packed into infinite chains through intermolecular O—H...O and N—H...O hydrogen bonds.

  12. Synthesis and structure of heptaaqua(nitrilotris(methylenephosphonato))(dibarium)sodium monohydrate [Na(H{sub 2}O){sub 3}(μ{sup 6}-NH(CH{sub 2}PO{sub 3}){sub 3})(μ-H{sub 2}O){sub 3}Ba{sub 2}(H{sub 2}O)] · H{sub 2}O

    Energy Technology Data Exchange (ETDEWEB)

    Somov, N. V., E-mail: somov@phys.unn.ru [Lobachevsky State University of Nizhny Novgorod (Russian Federation); Chausov, F. F., E-mail: xps@ftiudm.ru [Russian Academy of Sciences, Physical–Technical Institute, Ural Branch (Russian Federation); Zakirova, R. M., E-mail: ftt@udsu.ru [Udmurt State University (Russian Federation)

    2017-03-15

    Crystals of the monohydrate form of heptaaqua(nitrilotris(methylenephosphonato))(dibarium) sodium [Na(H{sub 2}O{sub )3}(µ{sup 6}-NH(CH{sub 2}PO{sub 3}){sub 3})(µ-H{sub 2}O){sub 3}Ba{sub 2}(H{sub 2}O)] · H{sub 2}O are obtained; space group P2{sub 1}/c, Z = 4; a = 13.9117(10) Å, b = 11.54030(10) Å, and c = 24.1784(17) Å, ß = 148.785(18)°. The Na atom is coordinated octahedrally by one oxygen atom of a phosphonate group and five water molecules, including two bridging molecules. Ba atoms occupy two inequivalent crystallographic positions with coordination number eight and nine. The coordination spheres of both Ba atoms include two water molecules. Each ligand is bound to one Na atom and five Ba atoms forming three Ba–O–P–O and five Ba–O–P–C–N–C–P–O chelate cycles. In addition to the coordination bonds, molecules, including the solvate water molecule, are involved in hydrogen bonds in the crystal packing.

  13. Crystal structures of tetramethylammonium (2,2′-bipyridinetetracyanidoferrate(III trihydrate and poly[[(2,2′-bipyridine-κ2N,N′di-μ2-cyanido-dicyanido(μ-ethylenediamine(ethylenediamine-κ2N,N′cadmium(IIiron(II] monohydrate

    Directory of Open Access Journals (Sweden)

    Songwuit Chanthee

    2016-05-01

    Full Text Available The crystal structures of the building block tetramethylammonium (2,2′-bipyridine-κ2N,N′tetracyanidoferrate(III trihydrate, [N(CH34][Fe(CN4(C10H8N2]·3H2O, (I, and a new two-dimensional cyanide-bridged bimetallic coordination polymer, poly[[(2,2′-bipyridine-κ2N,N′di-μ2-cyanido-dicyanido(μ-ethylenediamine-κ2N:N′(ethylenediamine-κ2N,N′cadmium(IIiron(II] monohydrate], [CdFe(CN4(C10H8N2(C2H8N22]·H2O, (II, are reported. In the crystal of (I, pairs of [Fe(2,2′-bipy(CN4]− units (2,2′-bipy is 2,2′-bipyridine are linked together through π–π stacking between the pyridyl rings of the 2,2′-bipy ligands to form a graphite-like structure parallel to the ab plane. The three independent water molecules are hydrogen-bonded alternately with each other, forming a ladder chain structure with R44(8 and R66(12 graph-set ring motifs, while the disordered [N(CH34]+ cations lie above and below the water chains, and the packing is stabilized by weak C—H...O hydrogen bonds. The water chains are further linked with adjacent sheets into a three-dimensional network via O—H...O hydrogen bonds involving the lattice water molecules and the N atoms of terminal cyanide groups of the [Fe(2,2′-bipy(CN4]− building blocks, forming an R44(12 ring motif. Compound (II features a two-dimensional {[Fe(2,2′-bipy(CN4Cd(en2]}n layer structure (en is ethylenediamine extending parallel to (010 and constructed from {[Fe(2,2′-bipy(CN4Cd(en]}n chains interlinked by bridging en ligands at the Cd atoms. Classical O—H...N and N—H...O hydrogen bonds involving the lattice water molecule and N atoms of terminal cyanide groups and the N—H groups of the en ligands are observed within the layers. The layers are further connected via π–π stacking interactions between adjacent pyridine rings of the 2,2′-bipy ligands, completing a three-dimensional supramolecular structure.

  14. (E-N′-(3,4-Dimethoxybenzylidenenicotinohydrazide monohydrate

    Directory of Open Access Journals (Sweden)

    J. Josephine Novina

    2014-07-01

    Full Text Available In the title hydrated compound, C15H15N3O3·H2O, the nicotinohydrazide molecule adopts a trans conformation with respect to the C=N double bond. The dihedral angle between the benzene and pyridine rings is 5.10 (14°. In the crystal, the solvent water molecule acts as an acceptor, forming an N—H...O hydrogen bond supported by two C—H...O contacts. It also acts as a donor, forming bifurcated O—H...(O,O and O—H...N hydrogen bonds that combine with the former contacts to form zigzag chains of molecules along the c-axis direction. An additional O—H...O donor contact completes a set of six hydrogen bonds to and from the water molecule and connects it to a third nicotinohydrazide molecule. This latter contact combines with weaker C—H...O hydrogen bonds supported by a C—H...π contact to stack molecules along b in a three-dimensional network.

  15. 4-[3-(4-Methylpiperidin-1-ylpropanamido]benzenesulfonamide monohydrate

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    Hasan Türkmen

    2012-12-01

    Full Text Available In the title compound, C15H23N3O3S·H2O, the piperidine ring has a chair conformation. In the crystal, the sulfonamide molecules are linked by N—H...O hydrogen bonds, forming a layer parallel to (10-1. The layers are interconnected via N—H...Ow, Ow—H...N and Ow—H...O (w = water hydrogen bonds, forming a three-dimensional network.

  16. 2-Oxo-1,2-dihydroquinoline-4-carboxylic acid monohydrate

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    Yassir Filali Baba

    2016-06-01

    Full Text Available In the title compound, C10H7NO3·H2O, O—H...O hydrogen bonds involving the carboxyl groups, the keto groups and the lattice water molecules form stepped sheets approximately parallel to {010} which are tied together by pairwise N—H...O interactions. The asymmetric unit contains two independent quinolone derivatives and two water molecules, one of which is disordered over two positions, of equal occupancy.

  17. 2-Phenylimidazolium hemi(benzene-1,3-dicarboxylate monohydrate

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    Wen-Yu Zhang

    2011-08-01

    Full Text Available The asymmetric unit of the title compound, C9H9N2+·0.5C8H4O4−·H2O, contains one 2-phenylimidazolium cation, half a benzene-1,3-dicarboxylate anion and one water molecule. In the crystal, components are connected by N—H...O and O—H...O hydrogen-bonding interactions into a three-dimensional network.

  18. Ferromagnetic Long Range Ordering in Copper(2) Maleate Monohydrate.

    Science.gov (United States)

    1988-11-20

    thanks the Consejo Nacional de Ciencia y Tecnologia for a partial fellowship. 10 References 1a) SYNTHECO, Inc., 1920 Industrial Pike, Gastonia, N.C...Philadelphia, 1966; Chapter 3. 14) D. B. Losee and W. E. Hatfield, Phs e.i Q 1122 (1974). 15) y . Yamamoto, M. Matsuura, and T. Haseda, J. Phys.-Soc...Mal in the solid state recorded at room temperature. 12 (0 Vj) N 4W +C +~ 13 4P4 CYC CS) (SG) CS + 0 (0 + C, S+ + 06 + + + 3 CC, (( Y ) uo p1 3ubA 00 CL

  19. Cytogenetical Effect of Creatine Monohydrate in Vicia faba Root Tips

    International Nuclear Information System (INIS)

    Ali, A.A.M.; El-zahrani, N.H.; El-shamrani, S.M.

    2010-01-01

    The present study has been conducted to evaluate the creatine effect on the cellular behavior at mitosis of Vicia faba using four concentrations (1.50, 2, 2.50 and 3 g/ 100 ml) with three exposure times (6, 12, 24 hour). Marked reduction of mitotic index was recorded at all creatine treatments and this trait was affected by creatine concentration and exposure time. Unbalanced mitotic stages percentages were observed after all treatments whereas, prophase % was decreased in all treatments but the opposite was true for metaphase %. While, (ana-telo) phases % were either increased or decreased after creatine treatments. Alteration of DNA or RNA contents, were obtained at different treatments. On the other hand, abnormalities were shown at all treatments with an increase percentage by increasing creatine concentration and exposure time. The most common of these abnormalities were: stickiness, disturbed and C metaphase. In addition, laggards, multipolor, and bridges were observed in some treatments but with low percentage

  20. 5-Acetamido-1H-pyrazole-4-carboxamide monohydrate

    Directory of Open Access Journals (Sweden)

    Lhoussaine El Ghayati

    2016-06-01

    Full Text Available There are two independent molecules of the title carboxamide compound, C6H8N4O2·H2O, as well as two independent water molecules in the asymmetric unit. The two independent carboxamide molecules differ primarily in the relative orientations of the peripheral methyl and amino groups. Intramolecular N—H...O hydrogen bonds assist in determining the orientations of the acetamido substituents. The three-dimensional crystal packing is directed by a large network of O—H...O, N—H...O, C—H...O and C—H...N hydrogen bonds.

  1. 21 CFR 520.608 - Dicloxacillin sodium monohydrate capsules.

    Science.gov (United States)

    2010-04-01

    ... Section 520.608 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES... § 510.600 (c) of this chapter. (c) Conditions of use. Dogs—(1) Amount. 5 to 10 milligrams per pound of...-producing staphylococci sensitive to the drug. (3) Limitations. For the treatment of dogs only. Continue...

  2. 2-[2-Chloro-5-(trifluoromethylphenyl]hexahydropyrimidine monohydrate

    Directory of Open Access Journals (Sweden)

    Reza Kia

    2008-09-01

    Full Text Available The molecule of the title compound, C11H12ClF3N2·H2O, is a substituted hexahydropyrimidine. There are two crystallographically independent molecules (A and B and two water molecules in the asymmetric unit of the title compound. Intermolecular C—H...Cl (× 2, C—H...F, and C—H...N (× 2 hydrogen bonds generate S(5 ring motifs. The dihedral angle between the two benzene rings is 8.17 (11°. The F atoms in molecule B are disordered over four positions with refined site-occupancies of ca 0.35/0.19/0.29/0.17 for the four components. In the crystal structure, molecules are arranged into one-dimensional extended chains along the c axis and are further stacked along the a axis by directed four-membered O—H...O—H interactions, forming two-dimensional networks parallel to the ac plane. The short distances between the centroids of the benzene rings (3.8002–3.8327 Å indicate the existence of π–π interactions. In addition, the crystal structure is further stabilized by N—H...O, O—H...N (× 4, N—H...Cl and C—H...O (× 2 hydrogen-bonding interactions.

  3. Lithium manganese(II) diaqua-boro-phosphate monohydrate.

    Science.gov (United States)

    Zhuang, Rong-Chuan; Chen, Xue-Yun; Mi, Jin-Xiao

    2008-07-05

    The title compound, LiMn(H(2)O)(2)[BP(2)O(8)]·H(2)O, is built up of an open framework of helical borophosphate ribbons inter-connected by MnO(4)(H(2)O)(2) octa-hedra, forming one-dimensional channels along [001] occupied by Li(+) cations and disordered H(2)O mol-ecules (site occupancy 0.5). The Li cations reside in two partially occupied sites [occupancies = 0.42 (3) and 0.289 (13)] near the helices.

  4. 2-Amino-1-(2-carboxylatoethylpyrimidin-1-ium monohydrate

    Directory of Open Access Journals (Sweden)

    Christopher R. Sparrow

    2010-12-01

    Full Text Available In the title structure, C7H9N3O2·H2O, there are two formula units in the asymmetric unit. The molecule is a zwitterion, containing a quaternary N atom and a deprotonated carboxyl group, with C—O distances in the range 1.256 (2–1.266 (3 Å. The two independent molecules form a hydrogen-bonded R22(16 dimer about an approximate inversion center via N—H...O hydrogen bonds, with N...O distances of 2.766 (2 and 2.888 (2 Å. O—H...O hydrogen bonds involving the water molecules and additional N—H...O hydrogen bonds link these dimers, forming double chains.

  5. Redetermination of dipotassium trichloridostannate(II chloride monohydrate

    Directory of Open Access Journals (Sweden)

    Fei Ye

    2013-02-01

    Full Text Available The title compound, K2[SnCl3]Cl·H2O, is the prototype of some isostructural compounds of composition M2[SnX3]X·H2O (M = large monovalent cation; X = halogen. In comparison with a previous study based on photographic data [Kamenar & Grdenić (1962. J. Inorg. Nucl. Chem. 24, 1039–1045], its crystal structure has now been redetermined using CCD-based data in order to gain more accurate values for bond lengths and angles within the [SnCl3]− anion and to locate the H atoms. The [SnCl3]− anion has a trigonal–pyramidal shape and exhibits crystallographic mirror symmetry. With the exception of the K+ ion which is located on a general position, all other atoms are situated on crystallographic mirror planes. The coordination polyhedron of the cation may be described by means of nine atoms in the form of a monocapped square antiprism with seven typical K—Cl/O distances and two additional atoms at considerably longer distances. The positions of the H atoms of the water molecule (also lying on a crystallographic mirror plane could be determined and confirm the existence of a bifurcated O—H...Cl hydrogen bond to neighbouring Cl atoms.

  6. Cholesterol monohydrate nucleation in ultrathin films on water

    DEFF Research Database (Denmark)

    Rapaport, H.; Kuzmenko, I.; Lafont, S.

    2001-01-01

    The growth of a cholesterol crystalline phase, three molecular layers thick at the air-water interface, was monitored by grazing incidence x-ray diffraction and x-ray reflectivity. Upon compression, a cholesterol film transforms from a monolayer of trigonal symmetry and low crystallinity to a tri......The growth of a cholesterol crystalline phase, three molecular layers thick at the air-water interface, was monitored by grazing incidence x-ray diffraction and x-ray reflectivity. Upon compression, a cholesterol film transforms from a monolayer of trigonal symmetry and low crystallinity...... in pathological lipid deposits....

  7. Ionic Conductivity of Solid Lithium Iodide and its Monohydrate

    DEFF Research Database (Denmark)

    Poulsen, Finn Willy

    1981-01-01

    The solid electrolytes LiI, LiI,H2O and LiI,D2O have been characterized by ac- and dc-conductivity measurements. LiI exhibits two conductivity regions: an extrinsic below ≈ 180°C and an intrinsic above, with activation energies of 0.43±0.04 eV and 0.81±0.05 eV respectively. The room temperature c...... conductivities of the hydrates LiI,H2O and LiI,D2O are 6.6× 10−6 and 6.1×10−6 (Ω cm)−1 respectively. The activation energy for Li-ion motion in LiI,D2O is 0.66±0.05 eV....

  8. Poly[[diaqua-μ6-succinato-di-μ5-succinato-didysprosium(III] monohydrate

    Directory of Open Access Journals (Sweden)

    Wei Xu

    2011-07-01

    Full Text Available The title compound, {[Dy2(C4H4O43(H2O2]·H2O}n, is isostructural with other lanthanide succinates of the same formula. The DyIII atom is nine-coordinated in a tricapped trigonal–prismatic environment by eight O atoms, derived from six carboxylate groups and a water molecule. One of the independent succinate anions is located about a crystallographic inversion center and the uncoordinated water molecule lies on a twofold axis. The crystal structure comprises edge-shared DyO9 polyhedra linked by succinate bridges, forming a three-dimensional network architecture. Intra- and intermolecular O—H...O hydrogen bonds are present in the crystal structure.

  9. Synthesis and molecular structure of (monoaqua) oxovanadium (IV) thiosemicarbazide-diacetate monohydrate

    International Nuclear Information System (INIS)

    Gerbeleu, N.V.; Bologa, A.O.; Burshtein, I.F.; Filippova, I.G.; Kiosse, G.A.

    1986-01-01

    This paper describes the structure for a new complex of oxovanadium (IV) with H 2 L. This compound was obtained by mixing warm aqueous solutions containing 1.0 g VOSO 4 .2H 2 O and H 2 L at room temperature. The coordinates and the individual temperature factors of the basis atoms in the structure VOLH 2 O .H 2 O are presented. It is shown that the vanadium atom in both complexes has a distorted octahedral environment. The geometrical isomerism is accompanied by differences in the conformations of the molecular ligand. Two geometrical isomers of a previously unknown type are concurrently present in the VOLH 2 O structure. The formation of these isomers is made possible by the different arrangement of inequivalent branches of the organic ligand. This type of isomerism should be expected in the complexes of other metals with H 2 L and in the coordination compounds of metals with other B-type tripod ligands

  10. Poly[[aqua(μ5-3,4,5,6-tetracarboxycyclohexane-1,2-dicarboxylatostrontium] monohydrate

    Directory of Open Access Journals (Sweden)

    Pei-Chi Cheng

    2011-12-01

    Full Text Available In the title compound, {[Sr(C12H10O12(H2O]·H2O}n, the SrII ion is coordinated by six O atoms of five symmetry-related 3,4,5,6-tetracarboxycyclohexane-1,2-dicarboxylate ligands and one water molecule in a slightly distorted monocapped trigonal–prismatic environment. The ligands bridge the SrII ions, forming a two-dimensional structure. In the crystal, O—H...O hydrogen bonds further connect the structure into a three-dimensional network. The H atoms of two of the carboxyl groups were refined as half-occupancy.

  11. A third monoclinic polymorph of 3,4,5-trihydroxybenzoic acid monohydrate

    Directory of Open Access Journals (Sweden)

    Güneş Demirtaş

    2011-06-01

    Full Text Available The title compound, C7H6O5·H2O, is a new polymorph of the structures reported by Jiang et al. (2000 [Acta Cryst. C56, 594–595] and Okabe et al. (2001 [Acta Cryst. E57, o764–o766]. The gallic acid molecule is essentially planar (r.m.s. deviation = 0.550 Å. An intramolecular O—H...O hydrogen bond occurs in the gallic acid molecule, which is linked to the water molecule by a further O—H...O hydrogen bond. In the crystal, the components are linked by O—H...O hydrogen bonds. The hydrogen-bonding pattern differs from those reported for the previous polymorphs.

  12. cis-Difluoridobis(1,10-phenanthroline)chromium(III) perchlorate monohydrate

    DEFF Research Database (Denmark)

    Birk, Torben; Bendix, Jesper; Weihe, Högni

    2008-01-01

    The title complex, [CrF(2)(C(12)H(8)N(2))(2)]ClO(4)·H(2)O, displays a slightly distorted octa-hedral coordination geometry around the central chromium(III) ion. The Cr environment is composed of a cis arrangement of two 1,10-phenanthroline [average Cr(III)-N = 2.0726 (10) Å] and two fluoride [ave...

  13. (E-2-[4-(Diethylaminostyryl]-1-methylquinolin-1-ium 4-chlorobenzenesulfonate monohydrate

    Directory of Open Access Journals (Sweden)

    Suchada Chantrapromma

    2014-04-01

    Full Text Available The asymmetric unit of the title hydrated salt, C22H25N2+·C6H4ClO3S−·H2O, comprises two 2-[4-(diethylaminostyryl]-1-methylquinolin-1-ium cations, two 4-chlorobenzenesulfonate anions and two solvent water molecules. One ethyl group of both cations displays disorder over two positions in a 0.659 (2:0.341 (2 ratio in one molecule and in a 0.501 (2:0.499 (2 ratio in the other. The sulfonate group of one anion is also disordered over two positions in a 0.893 (7:0.107 (7 ratio. The dihedral angle between the mean plane of the quinolinium ring system and that of benzene ring is 10.57 (18° in one cation and 14.4 (2° in the other. In the crystal, cations, anions and water molecules are linked into chains along the [010] direction by O—H...Osulfonate hydrogen bonds, together with weak C—H...Osulfonate and C—H...Cl interactions. The cations are stacked by π–π interactions, with centroid–centroid distances in the range 3.675 (2–4.162 (3 Å.

  14. X-ray diffraction study of polycrystalline dipalmitoylcephalin and dipalmitoyllecithin monohydrate. 2

    International Nuclear Information System (INIS)

    Foerster, G.; Doerfler, H.D.; Sackmann, H.

    1982-01-01

    The comparison of lattice constants of 1,2-dimpalmitoyl-DL-phosphatidylethanolamine (cephalin) and 1,2-dipalmitoyl-DL-phosphatidylcholine (lecithin), chain packing and chain tilting, and the efficiency of space filling suggests a similar molecular conformation in the crystal phase C1 of both phospholipids. The chains order essentially perpendicular to the bilayer plane but the headgroups are packed parallel to it. (author)

  15. Bis(2,6-diaminopyridinium) bis(pyridine-2,6-dicarboxylato)zincate(II) monohydrate

    Czech Academy of Sciences Publication Activity Database

    Tabatabaee, M.; Thahriri, M.; Thahriri, Mo.; Dušek, Michal; Fejfarová, Karla

    2011-01-01

    Roč. 67, Part 6 (2011), m769-u1197 ISSN 1600-5368 Grant - others:AV ČR(CZ) AP0701 Program:Akademická prémie - Praemium Academiae Institutional research plan: CEZ:AV0Z10100521 Keywords : single-crystal x-ray study * T = 120 K * zinc complexes Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.347, year: 2011

  16. Preparation, solubility, infrared spectra and radiolysis of tetramethylammonium hydrogenselenate monohydrate and lithium tetramethylammonium selenate tetrahydrate

    Czech Academy of Sciences Publication Activity Database

    Havlíček, D.; Turek, L.; Plocek, Jiří; Mička, Z.

    2006-01-01

    Roč. 71, č. 3 (2006), s. 411-422 ISSN 0010-0765 Institutional research plan: CEZ:AV0Z40320502 Keywords : tetramethylammonium salts * hydrogenselenates * selenates Subject RIV: CA - Inorganic Chemistry Impact factor: 0.881, year: 2006

  17. N-{2-[2-(5-Methyl-1H-pyrazol-3-ylacetamido]phenyl}benzamide monohydrate

    Directory of Open Access Journals (Sweden)

    Karim Chkirate

    2017-02-01

    Full Text Available The asymmetric unit of the title compound, C19H18N4O2·H2O, comprises the U-shaped pyrazole derivative and a solvent water molecule. The molecular conformation is partly determined by an intramolecular N—H...O hydrogen bond. The crystal packing is directed by an extensive network of O—H...O, N—H...O, N—H...N and C—H...O hydrogen bonds together with C—H...π(ring contacts that generate a three-dimensional network.

  18. Potassium bis(carbonato-O,O')(ethylenediamine-N,N')cobaltate(III) monohydrate at 173 K.

    Science.gov (United States)

    Belai, N; Dickman, M H; Pope, M T

    2001-07-01

    The title salt, K[Co(C2H8N2)(CO3)2].H2O, consists of a distorted octahedral cobalt complex anion and a seven-coordinate potassium cation. Both metal atoms have crystallographic twofold symmetry, one C2 axis passing through the Co atom and C--C bond, and another along a short K--O (water) bond of 2.600 A (corrected for libration). The carbonate is bidentate to both cobalt and potassium and the water forms a hydrogen bond to a carbonate O atom.

  19. 21 CFR 524.1610 - Orbifloxacin, mometasone furoate monohydrate, and posaconazole suspension.

    Science.gov (United States)

    2010-04-01

    ... HEALTH AND HUMAN SERVICES (CONTINUED) ANIMAL DRUGS, FEEDS, AND RELATED PRODUCTS OPHTHALMIC AND TOPICAL.... 000061 in § 510.600(c) of this chapter. (c) Conditions of use in dogs—(1) Amount. For dogs weighing less than 30 lbs. instill 4 drops once daily into the ear canal. For dogs weighing 30 lbs. or more, instill...

  20. Negative linear compressibility and massive anisotropic thermal expansion in methanol monohydrate.

    Science.gov (United States)

    Fortes, A Dominic; Suard, Emmanuelle; Knight, Kevin S

    2011-02-11

    The vast majority of materials shrink in all directions when hydrostatically compressed; exceptions include certain metallic or polymer foam structures, which may exhibit negative linear compressibility (NLC) (that is, they expand in one or more directions under hydrostatic compression). Materials that exhibit this property at the molecular level--crystalline solids with intrinsic NLC--are extremely uncommon. With the use of neutron powder diffraction, we have discovered and characterized both NLC and extremely anisotropic thermal expansion, including negative thermal expansion (NTE) along the NLC axis, in a simple molecular crystal (the deuterated 1:1 compound of methanol and water). Apically linked rhombuses, which are formed by the bridging of hydroxyl-water chains with methyl groups, extend along the axis of NLC/NTE and lead to the observed behavior.

  1. 8-[(3-Phenyl-1,2,4-oxadiazol-5-ylmethoxy]quinoline monohydrate

    Directory of Open Access Journals (Sweden)

    Shu-Yuan Bai

    2013-07-01

    Full Text Available In the title compound, C18H13N3O2·H2O, the oxadiazole ring forms dihedral angles 7.21 (10 and 21.25 (11° with the quinoline and benzene rings, respectively. The crystal structure features O—H...N hydrogen bonds and is further consolidated by C—H...O hydrogen-bonding interactions involving the water molecule of hydration.

  2. Rare calcium oxalate monohydrate calculus attached to the wall of the renal pelvis.

    Science.gov (United States)

    Grases, Felix; Costa-Bauza, Antonia; Prieto, Rafael M; Saus, Carlos; Servera, Antonio; García-Miralles, Reyes; Benejam, Joan

    2011-04-01

    Most renal calculi can be classified using well-established criteria in a manner that reflects both composition and fine structure under specific pathophysiological conditions. However, when a large patient population is considered, rare renal calculi invariably appear, some of which have never been classified; careful study is required to establish stone etiology in such cases. The patient in the present case report formed two types of calculi. One was attached on the wall of the renal pelvis near the ureter and part of the calculus was embedded inside pelvic renal tissue. The calculus developed on an ossified calcification located in the pelvis tissue. Current knowledge on the development of calcification in soft tissues suggests a pre-existing injury as an inducer of its development. A mechanism of calculus formation is proposed. The second stone was a typical jack-stone calculus. © 2011 The Japanese Urological Association.

  3. (S-2-(2-Pyrrolidinio-1H-benzimidazol-3-ium dichloride monohydrate

    Directory of Open Access Journals (Sweden)

    Dai Jing

    2009-06-01

    Full Text Available In the title compound, C11H15N32+·2Cl−·H2O, one N atom of the imidazole ring and the N atom of the pyrrolidine ring are protonated. The crystal structure is stabilized by aromatic π–π interactions between the benzene rings of neighbouring benzimidazole systems [centroid–centroid duistance = 3.712 (2 Å]. The crystal structure is further stabilized by intermolecular N—H...Cl, O—H...Cl and N—H...O hydrogen bonds.

  4. Aqua{N-[1-(2-oxidophenylethylidene]-l-serinato}copper(II monohydrate

    Directory of Open Access Journals (Sweden)

    Qin-Long Peng

    2009-12-01

    Full Text Available In the title compound, [Cu(C11H11NO4(H2O]·H2O, each CuII ion is four-coordinated by one N and two O atoms from the tridentate Schiff base ligand, and by one O atom from the coordinated water molecule in a distorted square-planar geometry. Intermolecular O—H...O hydrogen bonds link complex molecules and solvent water molecules into flattened columns propagated in [100].

  5. Structures, Energetics, and IR Spectra of Monohydrated Inorganic Acids: Ab initio and DFT Study.

    Science.gov (United States)

    Kołaski, Maciej; Zakharenko, Aleksey A; Karthikeyan, S; Kim, Kwang S

    2011-10-11

    We carried out extensive calculations of diverse inorganic acids interacting with a single water molecule, through a detailed analysis of many possible conformations. The optimized structures were obtained by using density functional theory (DFT) and the second order Møller-Plesset perturbation theory (MP2). For the most stable conformers, we calculated the interaction energies at the complete basis set (CBS) limit using coupled cluster theory with single, double, and perturbative triple excitations [CCSD(T)]. The -OH stretching harmonic and anharmonic frequencies are provided as fingerprints of characteristic conformers. The zero-point energy (ZPE) uncorrected/corrected (ΔEe/ΔE0) interaction energies and the enthalpies/free energies (ΔHr/ΔGr at room temperature and 1 bar) are reported. Various comparisons are made between many diverse inorganic acids (HmXOn where X = B/N/P/Cl/Br/I, m = 1-3, and n = 0-4) as well as other simple inorganic acids. In many cases, we find that the dispersion-driven van der Waals interactions between X in inorganic acid molecules and O in water molecules as well as the X(+)···O(-) electrostatic interactions are important.

  6. Topotactic decomposition and crystal structure of white molybdenum trioxide--monohydrate: prediction of structure by topotaxy

    International Nuclear Information System (INIS)

    Oswald, H.R.; Guenter, J.R.; Dubler, E.

    1975-01-01

    Single crystals of the white MoO 3 . H 2 O modification (''α-molybdic acid'') were transformed by heating to 160 0 C into perfect pseudomorphs built up from oriented MoO 3 crystallites of known structure. From the mutual orientation relationship of the unit cells of both phases involved in this topotactic reaction, as determined by X-ray photographs, a model for the so far unknown crystal structure of white MoO 3 . H 2 O could be deduced. Independently, this structure was determined by X-ray diffractometer data then: space group P anti 1, a = 7.388, b = 3.700, c = 6.673 A, α = 107.8, β = 113.6, γ = 91.2 0 , Z = 2. The structure was solved from the Patterson function and refined until R = 0.088. It is built up from isolated double chains of strongly distorted [MoO 5 (H 2 O)]-octahedra sharing two common edges with each other. This result agrees well with the model derived from topotaxy, and it becomes evident how the MoO 3 lattice is formed through corner linking of the isolated double chains after the water molecules are removed. The study of topotactic phenomena seems rather generally applicable to deduce the main features of structures involved and for better understanding of structural relationships. (U.S.)

  7. Synthesis, structural, photoluminescence, vibrational and DFT investigation of the bis (4-aminopyridinium) tetrachloridocuprate(II) monohydrate

    International Nuclear Information System (INIS)

    Kessentini, A.; Belhouchet, M.; Suñol, J.J.; Abid, Y.; Mhiri, T.

    2014-01-01

    The crystals of the family of alkylammonuim tetrachloridocuprate (II), (C 5 H 7 N 2 ) 2 CuCl 4 H 2 O, have been grown, structurally characterized and their vibrational as well as optical properties been studied. A preliminary single crystal X-ray diffraction structural analysis has revealed that the title compound belongs to the monoclinic system with space group C2/c. Its unit cell dimensions are: a=8.454 (2) Å, b=14.279 (2) Å, c=14.363 (3) Å, β=95.813 (4)°, with Z=4 and its crystal structure was determined and refined down to R 1 =0.029 and wR 2 =0.080. The crystal lattice is composed of discrete [CuCl 4 ] 2− tetrahedra surrounded by 4-aminopyridinium cations and water molecules which are interconnected by means of hydrogen bonding contacts [N–H…Cl, O–H…Cl and N–H…O]. Furthermore, the room temperature IR and Raman spectra of the title compound were recorded and analyzed. The optimized molecular structure and the vibrational spectra were calculated by the density functional theory (DFT) method using the B3LYP function. The organic–inorganic hybrid crystal thin film can be easily prepared by spin-coating method from the ethanol solution of the (C 5 H 7 N 2 ) 2 CuCl 4 H 2 O perovskite and it showed characteristic absorptions of CuCl-based layered perovskite centered at 288 and 400 nm, as well as the photoluminescence peak at around 443 nm. The unaided-eye-detectable blue luminescence emission comes from the excitonic transition in the CuCl 4 anions. - Highlights: • A new hybrid compound (C 5 H 7 N 2 ) 2 CuCl 4 H 2 O was synthesized. • Vibrational properties were studied by IR and Raman spectroscopy and examined theoretically using the DFT/B3LYP/LanL2DZ level of theory. • The UV–vis spectrum shows two absorption peaks at 288 and at 400 nm. • This compound show a strong blue emission at 443 nm

  8. catena-Poly[bis-(sulfamethoxazolium) [[trichloridocadmate(II)]-μ-chlorido] monohydrate].

    Science.gov (United States)

    Subashini, Annamalai; Muthiah, Packianathan Thomas; Bocelli, Gabriele; Cantoni, Andrea

    2007-12-21

    In the title compound, {(C(10)H(12)N(3)O(3)S)(2)[CdCl(4)]·H(2)O}(n), the Cd(II) atom is five-coordinate with a distorted trigonal-bipyramidal geometry formed by chloride ions. The Cd atom and two of the Cl atoms lie on a mirror plane. The cation is protonated on the amino group N atom; it is not coordinated to cadmium, but is hydrogen bonded to the chlorido ligands. Each water mol-ecule bridges two chlorido ligands, generating ring motifs along the -Cd-Cl-Cd- chains. The isoxazole unit and the amide groups are linked through a pair of N-H⋯N hydrogen bonds. The crystal structure is stabilized by N-H⋯O, O-H⋯Cl, C-H⋯N, N-H⋯Cl and C-H⋯O hydrogen bonds.

  9. catena-Poly[bis(sulfamethoxazolium [[trichloridocadmate(II]-μ-chlorido] monohydrate

    Directory of Open Access Journals (Sweden)

    Annamalai Subashini

    2008-01-01

    Full Text Available In the title compound, {(C10H12N3O3S2[CdCl4]·H2O}n, the CdII atom is five-coordinate with a distorted trigonal–bipyramidal geometry formed by chloride ions. The Cd atom and two of the Cl atoms lie on a mirror plane. The cation is protonated on the amino group N atom; it is not coordinated to cadmium, but is hydrogen bonded to the chlorido ligands. Each water molecule bridges two chlorido ligands, generating ring motifs along the –Cd—Cl—Cd– chains. The isoxazole unit and the amide groups are linked through a pair of N—H...N hydrogen bonds. The crystal structure is stabilized by N—H...O, O—H...Cl, C—H...N, N—H...Cl and C—H...O hydrogen bonds.

  10. catena-Poly[bis­(sulfamethoxazolium) [[trichloridocadmate(II)]-μ-chlorido] monohydrate

    Science.gov (United States)

    Subashini, Annamalai; Muthiah, Packianathan Thomas; Bocelli, Gabriele; Cantoni, Andrea

    2008-01-01

    In the title compound, {(C10H12N3O3S)2[CdCl4]·H2O}n, the CdII atom is five-coordinate with a distorted trigonal–bipyramidal geometry formed by chloride ions. The Cd atom and two of the Cl atoms lie on a mirror plane. The cation is protonated on the amino group N atom; it is not coordinated to cadmium, but is hydrogen bonded to the chlorido ligands. Each water mol­ecule bridges two chlorido ligands, generating ring motifs along the –Cd—Cl—Cd– chains. The isoxazole unit and the amide groups are linked through a pair of N—H⋯N hydrogen bonds. The crystal structure is stabilized by N—H⋯O, O—H⋯Cl, C—H⋯N, N—H⋯Cl and C—H⋯O hydrogen bonds. PMID:21200590

  11. High-pressure structural and dielectric studies of the phase transition in lithium thallium tartrate monohydrate

    Czech Academy of Sciences Publication Activity Database

    Kamba, S.; Kulda, Jiří; Petříček, V.; McIntyre, G.; Kiat, JP.

    2002-01-01

    Roč. 14, č. 15 (2002), s. 4045-4055 ISSN 0953-8984 R&D Projects: GA AV ČR KSK1048102 Keywords : rochelle salt * soft-mode * litlC4H4O6-center-DOT-H20 Subject RIV: BG - Nuclear, Atomic and Molecular Physics, Colliders Impact factor: 1.775, year: 2002

  12. High-pressure structural and dielectric studies of the phase transitions in lithium thallium tartrate monohydrate

    Czech Academy of Sciences Publication Activity Database

    Kamba, Stanislav; Kulda, J.; Petříček, Václav; McIntyre, G.; Kiat, J. P.

    2002-01-01

    Roč. 14, č. 15 (2002), s. 4045-4054 ISSN 0953-8984 R&D Projects: GA ČR GA202/01/0612; GA AV ČR IAA1010213 Institutional research plan: CEZ:AV0Z1010914 Keywords : lithium thalim tartarate monohzdrate * phase transitions * neutrom diffraction Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.775, year: 2002

  13. N,N-Dimethyl-N-propyl-propan-1-aminium chloride monohydrate.

    Science.gov (United States)

    Kärnä, Minna; Lahtinen, Manu; Valkonen, Jussi

    2008-10-11

    The title compound, C(8)H(20)N(+)·Cl(-)·H(2)O, has been prepared by a simple one-pot synthesis route followed by anion exchange using resin. In the crystal structure, the cations are packed in such a way that channels exist parallel to the b axis. These channels are filled by the anions and water mol-ecules, which inter-act via O-H⋯Cl hydrogen bonds [O⋯Cl = 3.285 (3) and 3.239 (3) Å] to form helical chains. The cations are involved in weak inter-molecular C-H⋯Cl and C-H⋯O hydrogen bonds. The title compound is not isomorphous with the bromo or iodo analogues.

  14. N,N-Dimethyl-N-propyl?propan-1-aminium chloride monohydrate

    OpenAIRE

    K?rn?, Minna; Lahtinen, Manu; Valkonen, Jussi

    2008-01-01

    The title compound, C8H20N+·Cl−·H2O, has been prepared by a simple one-pot synthesis route followed by anion exchange using resin. In the crystal structure, the cations are packed in such a way that channels exist parallel to the b axis. These channels are filled by the anions and water molecules, which interact via O—H...Cl hydrogen bonds [O...Cl = 3.285 (3) and 3.239 (3) Å] to form helical chains. The cations are involved in weak intermolecular C...

  15. Potassium 3-formyl-[1,1′-biphenyl]-4-olate monohydrate

    Directory of Open Access Journals (Sweden)

    Ryoji Moriwaki

    2017-09-01

    Full Text Available The title salt, K+·C13H9O2−·H2O, was synthesized from 5-bromosalicylaldehyde and a phenylboronic acid derivative using the Suzuki–Miyaura cross-coupling reaction (Miyaura & Suzuki, 1979. In addition to the intermolecular interactions between the charged species, two O—H...O hydrogen bonds involving the isolated water molecules further stabilize the crystal packing of the title salt leading to the formation of a three-dimensional framework structure.

  16. Estimation of Ziprasidone Hydrochloride Monohydrate in Bulk and Capsules by Reverse Phase HPLC

    Directory of Open Access Journals (Sweden)

    B. Sudha Rani

    2006-01-01

    Full Text Available A reverse phase HPLC method is described for the determination of Ziprasidone HCl mono hydrate in bulk and pharmaceutical dosage forms. Chromatography was carried out on an ODS C18 column using a mixture of methanol and phosphate buffer (55:45v/v as the mobile phase at a flow rate of 1mL/min. Detection was carried out at 314nm. The retension time of the drug was 4.522 min. The method produced linear responses in the concentration range of 0.5-30 μg /mL of Ziprasidone HCl mono hydrate.The method was found to be applicable for determination of the drug in capsules.

  17. Potassium l-2-nitrimino-1,3-diazepane-4-carboxylate monohydrate

    Directory of Open Access Journals (Sweden)

    Harutyun A. Karapetyan

    2008-11-01

    Full Text Available The title compound, K+·C6H9N4O4−·H2O, crystallizes with the K atoms located on special positions related by pseudocentres of symmetry. Each K atom is coordinated by six O-atom donors. The N and water H atoms are involved in inter- and intramolecular N—H...O, N—H...N and O—H...O hydrogen bonding. The data indicate inversion twinning.

  18. l-2-Nitrimino-1,3-diazepane-4-carboxylic acid monohydrate

    Directory of Open Access Journals (Sweden)

    Harutyun A. Karapetyan

    2008-07-01

    Full Text Available The title compound, C6H10N4O4·H2O, crystallizes with two independent formula units in the asymmetric unit, their geometric parameters being quite similar. The conformations of the 1,3-diazepane rings are also similar and close to a twist-boat. All ten O- and N-bound H atoms are involved in hydrogen bonds, two of which are intra- and eight intermolecular linking crystallographically independent molecules, into a three-dimensional hydrogen-bonded network.

  19. 3-(Aminocarbonylpyridinium diaqua-bis(pyridine-2,6-dicarboxylatobismuthate(III monohydrate

    Directory of Open Access Journals (Sweden)

    Janet Soleimannejad

    2012-07-01

    Full Text Available The asymmetric unit of the ionic title compound, (C6H7N2O[Bi(C7H3NO42(H2O2]·H2O or (acpyH[Bi(pydc2(H2O2]·H2O, contains an [Bi(pydc2(H2O2]− anion (where pydcH2 is pyridine-2,6-dicarboxylic acid, a protonated 3-(aminocarbonylpyridine as counter-ion, (acpyH+, and one uncoordinated water molecule. The anion is an eight-coordinate complex with a square-antiprismatic geometry around the BiIII atom. In the crystal, extensive O—H...O and N—H...O hydrogen bonds, as well as ion pairing, C=O...π interactions [O...centroid distance = 3.583 (5 Å], π–π stacking [centroid–centroid distance = 3.864 (3 Å], and C—H...π and C—H...O interactions, play an important role in the formation and stabilization of the three-dimensional supramolecular structure.

  20. 2,2′-[Biphenyl-2,2′-diylbis(oxy]diacetic acid monohydrate

    Directory of Open Access Journals (Sweden)

    Kuldip Singh

    2008-10-01

    Full Text Available In the crystal structure of the title compound, C16H14O6·H2O, the dihedral angle between the benzene rings is 60.8 (3°. Molecules are linked through a bifurcated O—H...O hydrogen bond, forming a zigzag chain along the b axis. The chains are further linked by O—H...O hydrogen bonds mediated by water molecules.

  1. Vibrational, calorimetric and nonlinear optical studies of melaminium-bis(trichloroacetate) monohydrate molecular ionic crystal

    Science.gov (United States)

    Debrus, S.; Marchewka, M. K.; Drozd, M.; Ratajczak, H.

    2007-04-01

    The efficiency of second harmonic generation for melaminium bis(trichloroacetate) was estimated relatively to KDP: deff = 3.09 deff (KDP). Room temperature FT IR and FT Raman spectra were recorded. Some spectral features of this new crystal are referred to corresponding one for melamine crystal as well as for other trichloroacetates. Differential scanning calorimetric measurements performed on powder sample indicate the phase transition point at approximately 276 and 239 K for heating and cooling, respectively.

  2. Dehydration of Sodium Carbonate Decahydrate to Monohydrate in a Fluidized Bed

    Czech Academy of Sciences Publication Activity Database

    Hartman, Miloslav; Veselý, Václav; Svoboda, Karel; Trnka, Otakar; Beran, Z.

    2001-01-01

    Roč. 47, č. 10 (2001), s. 2333-2340 ISSN 0001-1541 R&D Projects: GA ČR GA203/98/0101; GA AV ČR IAA4072711 Institutional research plan: CEZ:AV0Z4072921 Keywords : gas-solid reactions * sulfur-dioxide * thermal dehydration Subject RIV: CI - Industrial Chemistry, Chemical Engineering Impact factor: 1.793, year: 2001

  3. Synthesis, structural, photoluminescence, vibrational and DFT investigation of the bis (4-aminopyridinium) tetrachloridocuprate(II) monohydrate

    Energy Technology Data Exchange (ETDEWEB)

    Kessentini, A., E-mail: kessentiniabir@gmail.com [Laboratoire Physico-Chimie de l’Etat Solide, Département de Chimie, Faculté des Sciences de Sfax, Université de Sfax, B. P. 1171, 3000 Sfax (Tunisia); Belhouchet, M. [Laboratoire Physico-Chimie de l’Etat Solide, Département de Chimie, Faculté des Sciences de Sfax, Université de Sfax, B. P. 1171, 3000 Sfax (Tunisia); Suñol, J.J. [Departamento De Fisica, Universita de Girona, Compus Montilivi, Girona 17071 (Spain); Abid, Y. [Laboratoire de Physique appliquée, Faculté des Sciences de Sfax, Université de Sfax, B. P. 1171, 3000 Sfax (Tunisia); Mhiri, T. [Laboratoire Physico-Chimie de l’Etat Solide, Département de Chimie, Faculté des Sciences de Sfax, Université de Sfax, B. P. 1171, 3000 Sfax (Tunisia)

    2014-05-01

    The crystals of the family of alkylammonuim tetrachloridocuprate (II), (C{sub 5}H{sub 7}N{sub 2}){sub 2}CuCl{sub 4}H{sub 2}O, have been grown, structurally characterized and their vibrational as well as optical properties been studied. A preliminary single crystal X-ray diffraction structural analysis has revealed that the title compound belongs to the monoclinic system with space group C2/c. Its unit cell dimensions are: a=8.454 (2) Å, b=14.279 (2) Å, c=14.363 (3) Å, β=95.813 (4)°, with Z=4 and its crystal structure was determined and refined down to R{sub 1}=0.029 and wR{sub 2}=0.080. The crystal lattice is composed of discrete [CuCl{sub 4}]{sup 2−} tetrahedra surrounded by 4-aminopyridinium cations and water molecules which are interconnected by means of hydrogen bonding contacts [N–H…Cl, O–H…Cl and N–H…O]. Furthermore, the room temperature IR and Raman spectra of the title compound were recorded and analyzed. The optimized molecular structure and the vibrational spectra were calculated by the density functional theory (DFT) method using the B3LYP function. The organic–inorganic hybrid crystal thin film can be easily prepared by spin-coating method from the ethanol solution of the (C{sub 5}H{sub 7}N{sub 2}){sub 2}CuCl{sub 4}H{sub 2}O perovskite and it showed characteristic absorptions of CuCl-based layered perovskite centered at 288 and 400 nm, as well as the photoluminescence peak at around 443 nm. The unaided-eye-detectable blue luminescence emission comes from the excitonic transition in the CuCl{sub 4} anions. - Highlights: • A new hybrid compound (C{sub 5}H{sub 7}N{sub 2}){sub 2}CuCl{sub 4}H{sub 2}O was synthesized. • Vibrational properties were studied by IR and Raman spectroscopy and examined theoretically using the DFT/B3LYP/LanL2DZ level of theory. • The UV–vis spectrum shows two absorption peaks at 288 and at 400 nm. • This compound show a strong blue emission at 443 nm.

  4. N-(4-Chloro-1,3-benzothiazol-2-yl-2-(3-methylphenylacetamide monohydrate

    Directory of Open Access Journals (Sweden)

    H. S. Yathirajan

    2011-10-01

    Full Text Available In the title compound, C16H13ClN2OS·H2O, the dihedral angle between the mean planes of the benzothiazole ring system and the methylphenyl ring is 79.3 (6°. The crystal packing features intermolecular O—H...N, O—H...O and N—H...O hydrogen bonds involving the water molecule and weak C—H...O, C—H...Cg and π–π stacking interactions [centroid–centroid distances = 3.8743 (7, 3.7229 (7 and 3.7076 (8 Å].

  5. N-tert-Butyl-3-hydroxy-5-androstene-17-carboxamide monohydrate

    Directory of Open Access Journals (Sweden)

    Jiang-Sheng Li

    2009-07-01

    Full Text Available In the title compound, C24H39NO2·H2O, the A and C rings of the pregnolene derivative sterol adopt chair conformations, with the B ring in a flattened chair conformation and the five-membered ring in an envelope conformation twisted about the C/D ring junction. The N-tert-butylcarboxamide substituent is equatorial. The 3β-hydroxy H atom and one H atom of the water molecule are disordered over two positions with equal occupancies. In the crystal structure, O—H...O hydrogen bonds between the 3β-hydroxy groups of neighbouring molecules form dimers in the bc plane and these dimers are stacked along the a axis by additional O—H...O hydrogen bonds involving the water molecules. The steric effect of the bulky tert-butyl substituent in the carboxamide chain precludes hydrogen-bond formation by the N—H group.

  6. Gas-phase spectroscopy of protonated adenine, adenosine 5′-monophosphate and monohydrated ions

    DEFF Research Database (Denmark)

    Pedersen, S.O.; Støchkel, K.; Byskov, C.S.

    2013-01-01

    . The yields of these were measured as a function of the wavelength of the light from 210 nm to 300 nm, and they were combined to obtain the total photoinduced dissociation at each wavelength (i.e., action spectrum). A broad band between 230 nm and 290 nm and the tail of a band with maximum below 210 nm (high......-energy band) are seen. In the case of AdeH+(H2O), the dominant dissociation channel after photoexcitation in the low-energy band was simply loss of H2O while photodissociation of protonated AMP revealed two dominant dissociation channels associated with the formation of either AdeH+ or loss of H3PO4....... The action spectra of AdeH+, AdeH+(H2O), and AMPH+ are almost identical in the 230–290 nm region, and they resemble the absorption spectrum of protonated adenine in aqueous solution recorded at low pH. Hence from our work it is firmly established that the lowest-energy transitions are independent...

  7. 75 FR 16346 - Ophthalmic and Topical Dosage Form New Animal Drugs; Orbifloxacin, Mometasone Furoate Monohydrate...

    Science.gov (United States)

    2010-04-01

    ... posaconazole for the treatment of otitis externa in dogs. DATES: This rule is effective April 1, 2010. FOR... posaconazole) Otic Suspension for the treatment of otitis externa in dogs associated with susceptible strains... statement is required. Under section 512(c)(2)(F)(ii) of the Federal Food, Drug, and Cosmetic Act (21 U.S.C...

  8. Poly[[diaqua-μ(6)-succinato-di-μ(5)-succinato-didysprosium(III)] mono-hydrate].

    Science.gov (United States)

    Xu, Wei; Chang, Hai-Sheng; Guo, Xia-Xia

    2011-07-01

    The title compound, {[Dy(2)(C(4)H(4)O(4))(3)(H(2)O)(2)]·H(2)O}(n), is isostructural with other lanthanide succinates of the same formula. The Dy(III) atom is nine-coordinated in a tricapped trigonal-prismatic environment by eight O atoms, derived from six carboxyl-ate groups and a water mol-ecule. One of the independent succinate anions is located about a crystallographic inversion center and the uncoordinated water mol-ecule lies on a twofold axis. The crystal structure comprises edge-shared DyO(9) polyhedra linked by succinate bridges, forming a three-dimensional network architecture. Intra- and inter-molecular O-H⋯O hydrogen bonds are present in the crystal structure.

  9. catena-Poly[[[diaqua(1,10-phenanthrolinemanganese]-μ-3-[3-(carboxylatomethoxyphenyl]acrylato] monohydrate

    Directory of Open Access Journals (Sweden)

    Jun Ji

    2012-07-01

    Full Text Available The title compound, [Mn(C11H8O5(C12H8N2(H2O2]·H2O, was obtained under hydrothermal conditions. The coordination environment of the Mn(II atom is a distorted MnN2O4 octahedron defined by two N atoms from 1,10-phenanthroline, two water O atoms and two carboxylate O atoms from two acrylate anions. The bis-monodentate coordination mode of the anion leads to the formation of chains propagating in [010]. Intermolecular O—H...O hydrogen bonds link the chains into a two-dimensional network parallel to (100. In the voids of this arrangement, disordered lattice water molecules are present.

  10. Bis(di-2-pyridylamine-κ2N2,N2'platinum(II dibromide monohydrate

    Directory of Open Access Journals (Sweden)

    Kwang Ha

    2012-04-01

    Full Text Available The asymmetric unit of the title compound, [Pt(C10H9N32]Br2·H2O, contains two crystallographically independent half-molecules of the cationic PtII complex, two Br− anions and a lattice water molecule; an inversion centre is located at the centroid of each complex. Each PtII ion is four-coordinated in an essentially square-planar environment by four pyridine N atoms derived from the two chelating di-2-pyridylamine (dpa ligands, and the PtN4 unit is exactly planar. The chelate ring formed by the dpa ligand displays a boat conformation, with dihedral angles between the pyridine rings of 35.9 (2 and 41.0 (2°. The complex cations, Br− anions and solvent water molecules are linked by O—H...Br, N—H...Br, C—H...O and C—H...Br hydrogen bonds, forming a three-dimensional network.

  11. CCDC 961393: Experimental Crystal Structure Determination : 3-(Adamantan-1-yl)-1-mesityl-1H-imidazol-3-ium chloride monohydrate

    KAUST Repository

    Queval, Pierre; Jahier, Claire; Rouen, Mathieu; Artur, Isabelle; Legeay, Jean-Christophe; Falivene, Laura; Toupet, loic; Cré visy, Christophe; Cavallo, Luigi; Basle, Olivier; Mauduit, Marc

    2014-01-01

    An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

  12. Pomaglumetad Methionil (LY2140023 Monohydrate and Aripiprazole in Patients with Schizophrenia: A Phase 3, Multicenter, Double-Blind Comparison

    Directory of Open Access Journals (Sweden)

    David H. Adams

    2014-01-01

    Full Text Available We tested the hypothesis that long-term treatment with pomaglumetad methionil would demonstrate significantly less weight gain than aripiprazole in patients with schizophrenia. In this 24-week, multicenter, randomized, double-blind, Phase 3 study, 678 schizophrenia patients were randomized to either pomaglumetad methionil (n=516 or aripiprazole (n=162. Treatment groups were also compared on efficacy and various safety measures, including serious adverse events (SAEs, discontinuation due to adverse events (AEs, treatment-emergent adverse events (TEAEs, extrapyramidal symptoms (EPS, and suicide-related thoughts and behaviors. The pomaglumetad methionil group showed significantly greater weight loss at Week 24 (Visit 12 compared with the aripiprazole group (−2.8 ± 0.4 versus 0.4 ± 0.6; P<0.001. However, change in Positive and Negative Syndrome Scale (PANSS total scores for aripiprazole was significantly greater than for pomaglumetad methionil (−15.58 ± 1.58 versus −12.03 ± 0.99; P=0.045. The incidences of SAEs (8.2% versus 3.1%; P=0.032 and discontinuation due to AEs (16.2% versus 8.7%; P=0.020 were significantly higher for pomaglumetad methionil compared with aripiprazole. No statistically significant differences in the incidence of TEAEs, EPS, or suicidal ideation or behavior were noted between treatment groups. In conclusion, long-term treatment with pomaglumetad methionil resulted in significantly less weight gain than aripiprazole. This trial is registered with ClinicalTrials.gov NCT01328093.

  13. (Carbonato-κO,O')bis-(1,10-phenan-throline-κN,N')cobalt(III) nitrate monohydrate.

    Science.gov (United States)

    Andaç, Omer; Yolcu, Zuhal; Büyükgüngör, Orhan

    2009-12-12

    The crystal structure of the title compound, [Co(CO(3))(C(12)H(8)N(2))(2)]NO(3)·H(2)O, consists of Co(III) complex cations, nitrate anions and uncoordinated water mol-ecules. The Co(III) cation is chelated by a carbonate anion and two phenanthroline ligands in a distorted octa-hedral coordination geometry. A three-dimensional supra-molecular structure is formed by O-H⋯O and C-H⋯O hydrogen bonding, C-H⋯π and aromatic π-π stacking [centroid-centroid distance = 3.995 (1)Å] inter-actions.

  14. Bis{2-[(pyridin-2-ylmethylideneamino]benzoato-κ3N,N′,O}chromium(III nitrate monohydrate

    Directory of Open Access Journals (Sweden)

    Elena A. Buvaylo

    2014-04-01

    Full Text Available The title complex salt hydrate, [Cr(C13H9N2O22]NO3·H2O, comprises discrete cations, nitrate anions and solvent water molecules. The CrIII atom is octahedrally coordinated by two anionic Schiff base ligands with the O atoms being cis. The two ligands differ significantly with dihedral angles between the pyridine and benzene rings of 4.8 (2 and 24.9 (2°. The nitrate anion and solvent water molecule were modelled as being disordered, with the major components having site-occupancy values of 0.856 (14 and 0.727 (16, respectively. The crystal is built of alternating layers of cations and of anions plus water molecules, stacked along the c axis.

  15. Structural studies on the actinide carboxylates. 4. The crystal and molecular structure of succinate dioxouranium(VI) monohydrate

    Energy Technology Data Exchange (ETDEWEB)

    Bombieri, G; Benetollo, F [Consiglio Nazionale delle Ricerche, Padua (Italy). Lab. di Chimica e Tecnologia dei Radioelementi; Del Pra, A; Rojas, R

    1979-01-01

    The structure of the title compound, UO/sub 2/(CH/sub 2/COO)/sub 2/.H/sub 2/O, has been determined from three-dimensional X-ray data. The crystals are orthorhombic, space group Pbcn with four formula units in a cell. The coordination geometry about the uranium atom is pentagonal bipyramidal. The uranyl ions are equatorially surrounded by one water oxygen and by four carboxylate oxygen atoms of different succinic ligands. Each ligand is shared by four uranyl units giving rise to a polymeric-like structure.

  16. 4-Benzyl-6-bromo-2-(4-methoxyphenyl-4H-imidazo[4,5-b]pyridine monohydrate

    Directory of Open Access Journals (Sweden)

    Y. Ouzidan

    2010-04-01

    Full Text Available The imidazopyridine fused ring in the title compound, C20H16BrN3O·H2O, is coplanar with the aromatic ring at the 2-position [dihedral angle = 5.2 (1°]. In the five-membered imidazo portion, the C—N bond whose C atom is also connected to the pyridine N atom has predominantly double-bond character [1.334 (2 Å] whereas the C—N bond whose atom is connected to the pyridine C atom has predominantly single-bond character [1.371 (2 Å]. The water molecule engages in hydrogen bonding with the latter N atom; it is also connected to a symmetry-related water molecule, generating a linear chain structure.

  17. 4-Allyl-6-bromo-2-phenyl-4H-imidazo[4,5-b]pyridine monohydrate

    Directory of Open Access Journals (Sweden)

    Younès Ouzidan

    2010-08-01

    Full Text Available In the molecule of the title compound, C15H12BrN3·H2O, the phenyl ring is coplanar with the imidazopyridine ring system [dihedral angle = 0.4 (1°]. The water molecule is disordered over two positions with occupancies of 0.58 (1 and 0.42 (1, and it is linked to the main molecule via an O—H...N hydrogen bond.

  18. (E-3-Propoxymethylidene-2,3-dihydro-1H-pyrrolo[2,1-b]quinazolin-9-one monohydrate

    Directory of Open Access Journals (Sweden)

    Burkhon Zh Elmuradov

    2010-05-01

    Full Text Available The title compound, C15H16N2O2·H2O, was synthesized via the alkylation of 3-hydroxymethylidene-2,3-dihydro-1H-pyrrolo[2,1-b]quinazolin-9-one with n-propyl iodide in the presence of sodium hydroxide. The organic molecule and the water molecule both lie on a crystallographic mirror plane. In the crystal structure, intermolecular O—H...O and O—H...N hydrogen bonds link the components into extended chains along [100].

  19. Hemi(4,4′-bipyridinium hexafluoridophosphate bis(4-aminobenzoic acid 4,4′-bipyridine monohydrate

    Directory of Open Access Journals (Sweden)

    Yi-Fan Luo

    2009-02-01

    Full Text Available In the title compound, 0.5C10H10N22+·PF6−·C10H8N2·2C7H7NO2·H2O, the cation is located on a center of symmetry. The crystal structure is determined by a complex three-dimensional network of intermolecular O—H...O, O—H...N, N—H...N and N—H...F hydrogen bonds. π–π stacking interactions between neighboring pyridyl rings are also present; the centroid–centroid distance is 3.643 (5 Å. The hexafluoridophosphate anion is disordered over two positions with site-occupancy factors of ca 0.6 and 0.4.

  20. N,N-Dimethyl-1H-pyrazolo[3,4-d]pyrimidin-4-amine monohydrate

    Directory of Open Access Journals (Sweden)

    Mohamed El Hafi

    2018-02-01

    Full Text Available The asymmetric unit of the title compound, C7H9N5·H2O, consists of two formula units differing slightly in the orientation of the dimethylamino groups. In the crystal, a combination of O—H...N and N—H...O hydrogen bonds involving the water molecules of crystallization, as well as slipped π-stacking interactions between pyrazolopyrimidine units form layers parallel to the bc plane.

  1. CCDC 949811: Experimental Crystal Structure Determination : bis(2,9-Dimethyl-1,10-phenanthroline)-copper hydrogen difluoride monohydrate

    KAUST Repository

    Liu, Yanpin

    2014-01-01

    An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

  2. Chlorido[1-diphenylphosphanyl-3-(phenylsulfanylpropane-κ2P,S](η5-pentamethylcyclopentadienyliridium(III chloride monohydrate

    Directory of Open Access Journals (Sweden)

    Gerd Ludwig

    2012-06-01

    Full Text Available The crystal structure of the title compound, [Ir(C10H15Cl(C21H21PS]Cl·H2O, consists of discrete [Ir(η5-C5Me5Cl{Ph2P(CH23SPh-κP,κS}]+ cations, chloride anions and water molecules. The IrIII atom is coordinated by an η5-C5Me5 ligand, a chloride and a Ph2P(CH23SPh-κP,κS ligand, leading to a three-legged piano-stool geometry. In the crystal, two water molecules and two chloride anions are linked by weak O—H...Cl hydrogen bonding into tetramers that are located on centers of inversion. The H atoms of one of the methyl groups are disordered and were refined using a split model.

  3. CCDC 949811: Experimental Crystal Structure Determination : bis(2,9-Dimethyl-1,10-phenanthroline)-copper hydrogen difluoride monohydrate

    KAUST Repository

    Liu, Yanpin; Chen, Chaohuang; Li, Huaifeng; Huang, Kuo-Wei; Tan, Jianwei; Weng, Zhiqiang

    2014-01-01

    An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from

  4. Crystal structure of bis[μ-bis(diphenylphosphanylmethane-κ2P:P′]digold(I dichloride acetone monosolvate monohydrate

    Directory of Open Access Journals (Sweden)

    Chien Ing Yeo

    2015-08-01

    Full Text Available In the title complex salt, [Au2{(C6H52PCH2P(C6H52}]Cl2·(CH32C=O·H2O, the dication forms an eight-membered {—PCPAu}2 ring with a transannular aurophilic interaction [Au...Au = 2.9743 (2 Å]. The ring approximates a flattened boat conformation, with the two methylene C atoms lying ca 0.58–0.59 Å above the least-squares plane defined by the Au2P4 atoms (r.m.s. deviation = 0.0849 Å. One Cl− anion functions as a weak bridge between the AuI atoms [Au...Cl = 2.9492 (13 and 2.9776 (12 Å]. The second Cl− anion forms two (waterO—H...Cl hydrogen bonds about a centre of inversion, forming a centrosymmetric eight-membered {...HOH...Cl}2 supramolecular square. Globally, the dications and loosely associated Cl− anions assemble into layers lying parallel to the ac plane, being connected by C—H...Cl,π(phenyl interactions. The supramolecular squares and solvent acetone molecules are sandwiched in the inter-layer region, being connected to the layers on either side by C—H...Cl,O(acetone interactions.

  5. The quantitative monitoring of mechanochemical reaction between solid L-tartaric acid and sodium carbonate monohydrate by terahertz spectroscopy

    Science.gov (United States)

    Liu, Xiaohong; Liu, Guifeng; Zhao, Hongwei; Zhang, Zengyang; Wei, Yongbo; Liu, Min; Wen, Wen; Zhou, Xingtai

    2011-11-01

    The solid-state reaction of chiral tartaric acid and alkali carbonate was studied by terahertz time-domain spectroscopy (THz-TDS). The sodium tartrate dihydrate was synthesized with high efficiency by mechanical grinding in the solid-state without waste that is particularly sustainable and environmentally benign. Distinct THz absorptions were observed for reactants and products. It indicates that THz spectroscopy is sensitive to different materials and crystal structures. The characteristic THz absorption peak at 1.09 THz of L (+)-Tartaric acid was selected for quantitative analysis. The reaction kinetics could be expressed by the Second-order equation and the Jander equation, which is consistent with a three-dimensional diffusion mechanism. The combination of multi-techniques including synchrotron radiation X-ray powder diffraction (SRXRPD), Fourier transform infrared (FT-IR) and scanning electron microscopy (SEM) was used to investigate the grinding process and presented supporting evidences. The results demonstrate that THz spectroscopy technique has great potential applications in process monitoring and analysis in pharmaceutical and chemical synthesis industry.

  6. μ-Oxalato-bis[(2,2′-bipyridylcopper(II] bis(perchlorate dimethylformamide disolvate monohydrate

    Directory of Open Access Journals (Sweden)

    Alexander N. Boyko

    2010-09-01

    Full Text Available The title compound, [Cu2(C2O4(C10H8N24](ClO42·2C3H7NO·H2O, contains doubly charged centrosymmetric dinuclear oxalato-bridged copper(II complex cations, perchlorate anions, and DMF and water solvate molecules. In the complex cation, the oxalate ligand is coordinated in a bis-bidentate bridging mode to the Cu atoms. Each Cu atom has a distorted tetragonal-bipyramidal environment, being coordinated by two N atoms of the two chelating bipy ligands and two O atoms of the doubly deprotonated oxalate anion. Pairs of perchlorate anions and water molecules are linked into rectangles by O—H...O bonds in which the perchlorate O atoms act as acceptors and the water molecules as donors. Methyl groups of the DMF solvent molecule are disordered over two sites with occupancies of 0.453 (7:0.547 (7, and the water molecule is half-occupied.

  7. Hydrothermal synthesis and structure of nickel(II) metavanadate monohydrate, NiV2O6.H2O

    International Nuclear Information System (INIS)

    Marcos, M.D.; Amoros, P.; Beltran-Porter, A.; Ramirez de Arellano, M.C.

    1995-01-01

    The structure of NiV 2 O 6 .H 2 O consists of infinite chains of [VO 4 ] tetrahedra running along the [100] direction connected by isolated [Ni 2 O 8 (H 2 O) 2 ] dimeric entities to build up a three-dimensional network. A valence-bond analysis allows the identification of the O atoms of the water molecules. (orig.)

  8. CCDC 1029960: Experimental Crystal Structure Determination : catena-[triethylammonium (mu-1,3,5-benzenetricarboxylato)-cobalt(ii) monohydrate

    KAUST Repository

    Lu, Hai-Sheng

    2014-01-01

    An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

  9. Tris(cyclohexylammonium cis-dichloridobis(oxalato-κ2O1,O2stannate(IV chloride monohydrate

    Directory of Open Access Journals (Sweden)

    Modou Sarr

    2013-11-01

    Full Text Available The crystal structure of the title compound, (C6H14N3[Sn(C2O42Cl2]Cl·H2O, contains three cyclohexylammonium cations, one stannate(IV dianion, one isolated chloride anion and one lattice water molecule. The cyclohexylammonium cations adopt chair conformations. In the complex anion, two bidentate oxalate ligands and two chloride anions in cis positions coordinate octahedrally to the central SnIV atom. The cohesion of the molecular entities is ensured by the formation of N—H...O, O—H...O, O—H...Cl and N—H...Cl interactions involving cations, anions and the lattice water molecule, giving rise to a layer-like arrangement parallel to (010.

  10. N-[5-Methyl-2-(2-nitrophenyl-4-oxo-1,3-thiazolidin-3-yl]pyridine-3-carboxamide monohydrate

    Directory of Open Access Journals (Sweden)

    Mehmet Akkurt

    2011-02-01

    Full Text Available In the title compound, C16H14N4O4S·H2O, the benzene and pyridine rings make a dihedral angle of 85.8 (1°. Both enantiomers of the chiral title compound are statistically disordered over the same position in the unit cell. The methyl and carbonyl group attached to the stereogenic center (C5 of the thiazolidine ring were therefore refined with common site-occupation factors of 0.531 (9 and 0.469 (9, respectively, for each stereoisomer. In the crystal, intermolecular N—H...O, O—H...O and O—H...N hydrogen bonds link the molecules, forming a three-dimensional supramolecular network. The crystal structure further shows π–π stacking interactions [centroid–centroid distance = 3.5063 (13 Å] between the pyridine rings.

  11. From dihydrated iron(III) phosphate to monohydrated ammonium-iron(II) phosphate: Solvothermal reaction mediated by acetone-urea mixtures

    Energy Technology Data Exchange (ETDEWEB)

    Alfonso, Belen F., E-mail: mbafernandez@uniovi.es [Departamento de Fisica, Universidad de Oviedo, Calvo Sotelo, s/n 33007 Oviedo (Spain); Trobajo, Camino [Departamento de Quimica Organica e Inorganica, Universidad de Oviedo-CINN, Julian Claveria 8, 33006 Oviedo (Spain); Pique, Carmen [Departamento de Fisica, Universidad de Oviedo, Calvo Sotelo, s/n 33007 Oviedo (Spain); Garcia, Jose R. [Departamento de Quimica Organica e Inorganica, Universidad de Oviedo-CINN, Julian Claveria 8, 33006 Oviedo (Spain); Blanco, Jesus A. [Departamento de Fisica, Universidad de Oviedo, Calvo Sotelo, s/n 33007 Oviedo (Spain)

    2012-12-15

    By reaction between synthetic phosphosiderite FePO{sub 4}{center_dot}2H{sub 2}O, urea (NH{sub 2}){sub 2}CO, and acetone (CH{sub 3}){sub 2}CO, we report a novel solvothermal synthesis of polycrystalline NH{sub 4}FePO{sub 4}{center_dot}H{sub 2}O. The preparation of other two individual phases, NH{sub 4}Fe{sub 2}(OH)(PO{sub 4}){sub 2}{center_dot}2H{sub 2}O and NH{sub 4}Fe{sub 2}(PO{sub 4}){sub 2}, is also described. The obtained product is a function of the reaction time and the N/P molar ratio in the reagent mixture, and the existence of structural memory in the dissolution-precipitation processes is discussed. Below 25 K, NH{sub 4}FePO{sub 4}{center_dot}H{sub 2}O behaves magnetically in a complex way, because both ferromagnetic and antiferromagnetic signals are superimposed, suggesting the existence of a canting of iron(II) magnetic moments. - Graphical abstract: Solvothermal synthesis of polycrystalline NH{sub 4}FePO{sub 4}{center_dot}H{sub 2}O is presented. The preparation of other two individual phases, NH{sub 4}Fe{sub 2}(OH)(PO{sub 4}){sub 2}{center_dot}2H{sub 2}O and NH{sub 4}Fe{sub 2}(PO{sub 4}){sub 2} as a function of the N/P molar ratio in the reagent mixture and the reaction time, is also described. Highlights: Black-Right-Pointing-Pointer Solvothermal synthesis of NH{sub 4}FePO{sub 4}{center_dot}H{sub 2}O from an Fe(III) phosphate: reduction process. Black-Right-Pointing-Pointer Formation of two intermediate metastable phases: phase diagram. Black-Right-Pointing-Pointer Thermal decomposition in two steps: mass loss of both water and ammonia. Black-Right-Pointing-Pointer Magnetic behaviour: AF+constant spontaneous magnetization.

  12. {4-Phenyl-1-[1-(1,3-thiazol-2-ylethylidene]thiosemicarbazidato}{4-phenyl-1-[1-(1,3-thiazol-2-ylethylidene]thiosemicarbazide}nickel(II chloride monohydrate

    Directory of Open Access Journals (Sweden)

    Ramaiyer Venkatraman

    2010-05-01

    Full Text Available In the title compound, [Ni(C12H11N4S2(C12H12N4S2]Cl·H2O, the NiII ion is chelated by two 2-acetylthiazole-3-phenylthiosemicarbazone ligands, forming a distorted octahedral complex. The metal ion is coordinated via the thiazole nitrogen, imine nitrogen and thione sulfur atoms from each thiosemicarbazone ligand, and two coordinating units lie almost perpendicular to each other give dihedral angle = 81.89 (1°]. One thiosemicarbazone unit is found to bind a chloride anion through two hydrogen bonds, while the other is linked with the disordered crystal water molecule. Two molecules are connected to each other through an intermolecular N—H...S interaction, forming a centrosymmetric dimer. Dimers are linked into sheets by π–π stacking of two phenyl rings [shortest C...C distance = 4.041 (3 Å].

  13. catena-Poly[[[diaqua(2-fluorobenzoato-κ2O,O′strontium]-μ3-2-fluorobenzoato-κ5O:O,O′:O′,F] monohydrate

    Directory of Open Access Journals (Sweden)

    Zhu-Nian Jin

    2011-04-01

    Full Text Available In the title compound, {[Sr(C7H4FO22(H2O2]·H2O}n, the SrII atom is coordinated by six O atoms and one F atom from four 2-fluorobenzoate ligands and two water molecules, resulting in an irregular SrFO8 coordination environment. The μ3-2-fluorobenzoate ligand bridges three symmetry-related SrII atoms, giving rise to a chain structure extending along [010]. The polymeric chains are connected via O—H...O hydrogen bonds into a two-dimensional supramolecular structure parallel to (100.

  14. Crystal structure of tris(1,10-phenanthroline-κ2N,N′iron(II bis[bis(trifluoromethylsulfonylimide] monohydrate

    Directory of Open Access Journals (Sweden)

    Kazunori Teramoto

    2015-01-01

    Full Text Available The crystal structure of the title complex, [Fe(C12H8N23][(CF3SO22N]2·H2O, is constructed by one octahedral [Fe(phen3]2+ (phen = 1,10-phenanthroline cation (point group symmetry 2, two Tf2N− [bis(trifluoromethylsulfonylimide] anions, and one water molecule of crystallization (point group 2. The Fe—N bond lengths are indicative of a d6 low-spin state for the FeII ion in the complex. The dihedral angle between the phen ligands in the cation is 87.64 (6°. The Tf2N− counter-anion is non-coordinating, with the –CF3 groups arranged in a trans fashion with respect to each other, leading to an anti,anti conformation of the –CF3 groups and –SO2N– moieties relative to the S—C bonds. The water molecule of crystallization connects two O atoms of the Tf2N− anions through weak hydrogen bonds. C—H...O hydrogen-bonding interactions are also observed, consolidating the packing of the molecules into a three-dimensional network structure.

  15. rac-6-Hydroxy-4-(4-nitrophenyl-5-(2-thienylcarbonyl-6-(trifluoromethyl-3,4,5,6-tetrahydropyrimidin-2(1H-one monohydrate

    Directory of Open Access Journals (Sweden)

    Jian-Li Zhang

    2010-11-01

    Full Text Available The title compound, C16H12F3N3O5S·H2O, was prepared by reaction of 4-nitrobenzaldehyde, 4,4,4-trifluoro-1-(thiophen-2-ylbutane-1,3-dione and urea. The asymmetric unit contains two independent molecules, with essentially identical geometries and conformations. The dihydropyrimidine rings adopt a half-chair conformation. The dihedral angles between the benzene ring and the thiophene ring are 54.82 (8 and 58.72 (8° in the two molecules. The molecular conformation of one of the molecules is stabilized by two intramolecular O—H...O hydrogen bonds, generating an S(6 ring. The crystal structure is stabilized by intermolecular O—H...O and N—H...O hydrogen bonds.

  16. 3-{2-[(3-{(E-2-[4-(Dimethylaminophenyl]ethenyl}quinoxalin-2-yloxy]ethyl}-1,3-oxazolidin-2-one monohydrate

    Directory of Open Access Journals (Sweden)

    Youssef Ramli

    2012-01-01

    Full Text Available In the title compound, C23H24N4O3·H2O, the 1,3-oxazoline ring is nearly planar [maximum deviation = 0.059 (2 Å] and its mean plane is twisted by 30.12 (8° with respect to the quinoxaline fused-ring system; the benzene ring is nearly coplanar with the quinoxaline fused-ring system [dihedral angle = 2.52 (2°]. The water molecule of crystallization is hydrogen-bond donor to an N atom of the quinoxaline ring system as well as an O atom of the oxazolinone unit, the two hydrogen bonds generating a chain running along the c axis.

  17. Crystal structure of 2-amino-1,3-dibromo-6-oxo-5,6-dihydropyrido[1,2-a]quinoxalin-11-ium bromide monohydrate

    Directory of Open Access Journals (Sweden)

    Md. Serajul Haque Faizi

    2015-11-01

    Full Text Available In the title hydrated salt, C12H8Br2N3O+·Br−·H2O, which was synthesized by the reaction of the pyridine derivative Schiff base N1,N4-bis(pyridine-2-ylmethylenebenzene-1,4-diamine with bromine, the asymmetric unit contains a 2-amino-1,3-dibromo-6-oxo-5,6-dihydropyrido[1,2-a]quinoxalin-11-ium cation, with a protonated pyridine moiety, a bromide anion and a water molecule of solvation. The cation is non-planar with the dibromo-substituted benzene ring, forming dihedral angles of 24.3 (4 and 11.5 (4° with the fused pyridine and pyrazine ring moieties, respectively. In the crystal, the cations are linked through a centrosymmetric hydrogen-bonded cyclic R42(8 Br2(H2O2 unit by N—H...Br, N—H...O and O—H...Br hydrogen bonds, forming one-dimensional ribbons extending along b, with the planes of the cations lying parallel to (100.

  18. 4-(4-Chlorophenyl-6-hydroxy-5-(2-thienylcarbonyl-6-(trifluoromethyl-3,4,5,6-tetrahydropyrimidin-2(1H-one monohydrate

    Directory of Open Access Journals (Sweden)

    Mohammad Hossein Mosslemin

    2009-06-01

    Full Text Available The asymmetric unit of the title compound, C16H12ClF3N2O3S·H2O, contains two crystallographically independent organic molecules and two water molecules. The organic species are linked by an intermolecular O—H...O hydrogen bond, while the water molecules are connected to them through intermolecular O—H...N hydrogen bonds. The thiophene and phenyl rings are oriented at dihedral angles of 62.35 (4 in the first independent molecule and 60.74 (5° in the second, while the pyrimidine rings adopt twisted conformations in both molecules. Intramolecular N—H...F interactions result in the formation of two five-membered rings having envelope conformations. In the crystal structure, further intermolecular O—H...O and N—H...O hydrogen bonds link the molecules into chains.

  19. CCDC 961639: Experimental Crystal Structure Determination : 3-Cyclopropyl-1-(2,6-diisopropylphenyl)-1H-imidazol-3-ium chloride monohydrate

    KAUST Repository

    Queval, Pierre; Jahier, Claire; Rouen, Mathieu; Artur, Isabelle; Legeay, Jean-Christophe; Falivene, Laura; Toupet, loic; Cré visy, Christophe; Cavallo, Luigi; Basle, Olivier; Mauduit, Marc

    2014-01-01

    An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

  20. (Carbonato-κ2 O,O′)bis­(1,10-phenan­throline-κ2 N,N′)cobalt(III) nitrate monohydrate

    Science.gov (United States)

    Andaç, Ömer; Yolcu, Zuhal; Büyükgüngör, Orhan

    2010-01-01

    The crystal structure of the title compound, [Co(CO3)(C12H8N2)2]NO3·H2O, consists of CoIII complex cations, nitrate anions and uncoordinated water mol­ecules. The CoIII cation is chelated by a carbonate anion and two phenanthroline ligands in a distorted octa­hedral coordination geometry. A three-dimensional supra­molecular structure is formed by O—H⋯O and C—H⋯O hydrogen bonding, C—H⋯π and aromatic π–π stacking [centroid–centroid distance = 3.995 (1)Å] inter­actions. PMID:21579944

  1. [A study of the properties of tablets from mixtures of two size degrees of alpha-lactose monohydrate and microcrystalline cellulose].

    Science.gov (United States)

    Muzíková, J

    2006-03-01

    The paper examines the strength and disintegration time of compacts from the mixtures of two types of Tablettosas. Tablettosa 70 and Tablettosa 100 with microcrystalline cellulose represented by Vivapur 102. The mixtures of dry binders were prepared in the ratios of 3:1, 1:1, and 1:3. The effect of two concentrations of the lubricant magnesium stearate on the strength and disintegration time of compacts was also examined. Tablet strength increased with higher representation of microcrystalline cellulose in the mixture, and decreased with higher stearate concentration. The compacts from the mixtures with Tablettosa 100 showed higher strength. Disintegration time was highest in the compacts with the largest perccintage of microcrystalline cellulose, and longer in the case of the mixtures with Tablettosa 100. Stearate did not exert a negative effect on disintegration time. In the mixtures of Tablettosas with Vivapur 102 in a ratio of 1:1, the effect of the model active ingredient acetylsalicylic acid on the above-mentioned properties of tablets was tested. acetylsalicylic acid produced a further decrease in the strength of compacts and shortened the disintegration time in more instances in the cased of the mixtures with Tahlettosa 100.

  2. Evaluation of the effects of Citrus sinensis seed oil on blood glucose, lipid profile and liver enzymes in rats injected with alloxan monohydrate

    Directory of Open Access Journals (Sweden)

    K.C Chilaka

    2015-06-01

    Conclusions: However, further studies need to be carried out to show its mechanism of action and to isolate the active ingredient in the Citrus sinensis seed oil that is responsible for these actions.

  3. CCDC 928609: Experimental Crystal Structure Determination : catena-[(mu7-Biphenyl-2,4,4',6-tetracarboxylato)-triaqua-di-cadmium(ii) monohydrate

    KAUST Repository

    Lou, Xin-Hua

    2013-01-01

    An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

  4. Crystal structure of 2-hydroxy-N-(2-hydroxyethyl-N-{2-hydroxy-3-[(E-N-hydroxyethanimidoyl]-5-methylbenzyl}ethanaminium acetate monohydrate

    Directory of Open Access Journals (Sweden)

    Gary S. Nichol

    2015-03-01

    Full Text Available The structure of the title hydrated molecular salt, C14H23N2O4+·C2H3O2−·H2O, was determined as part of a wider study on the use of the molecule as a polydentate ligand in the synthesis of MnIII clusters with magnetic properties. The cation features intramolecular O—H...N and N—H...O hydrogen-bond interactions. The crystal structure features a range of intermolecular hydrogen-bonding interactions, principally O—H...O interactions between all three species in the asymmetric unit. An R24(8 graph-set hydrogen-bonding motif between the anion and water molecules serves as a unit which links to the cation via the diethanolamine group. Each O atom of the acetate anion accepts two hydrogen bonds.

  5. {2-[(2-Acetylhydrazin-1-ylidenemethyl-κ2N1,O]-6-methoxyphenolato-κO1}(nitrato-κOcopper(II monohydrate

    Directory of Open Access Journals (Sweden)

    Ibrahima Elhadj Thiam

    2010-02-01

    Full Text Available In the title complex, [Cu(C10H11N2O3(NO3]·H2O, prepared from the Schiff base N′-(3-methoxy-2-oxidobenzylideneacetohydrazide, the CuII atom is coordinated by two O atoms and one N atom from the ligand and one O atom from a nitrate group in a distorted square-planar geometry. The CuII atom has a weak interaction with another O atom of the nitrate group. The two O atoms of the tridentate Schiff base ligand are in a trans arrangement. O—H...O and N—H...O hydrogen bonds involving the uncoordinated water molecule are observed.

  6. Ethyl 4′-ethenyl-2′-oxo-4-phenyl-2-(3,4,5-trimethoxyphenylspiro[pyrrolidine-3,3′-indoline]-5-carboxylate monohydrate

    Directory of Open Access Journals (Sweden)

    P. Ramesh

    2008-11-01

    Full Text Available In the title compound, C31H32N2O6·H2O, the pyrrolidine ring adopts an envelope conformation. The ethyl C atoms of the ethoxycabonyl group are disordered over two positions with occupancies of ca 0.80 and 0.20. Intramolecular N—H...O hydrogen bonds form S(5 and S(6 ring motifs. Molecules are linked into a three-dimensional framework by O—H...O, N—H...O and C—H...O hydrogen bonds, and by C—H...π interactions.

  7. Poly[piperazine-1,4-diium [μ4-chlorido-μ3-chlorido-tri-μ2-chlorido-chloridodicadmate(II] monohydrate

    Directory of Open Access Journals (Sweden)

    Marwa Adib

    2012-02-01

    Full Text Available In the title compound, {(C5H14N2[Cd2Cl6]·H2O}n, the asymmetric unit contains one piperazinediium cation, one [Cd2Cl6]2− anion and a water molecule. The coordination geometries of the two Cd2+ cations are distorted octahedral. Adjacent CdII atoms are interconnected alternately by paired chloride bridges, generating polymeric chains parallel to [010]. Neighbouring chains are connected by O—H...Cl hydrogen bonds involving the water molecules, forming layers at z = n/2. The crystal packing is further stabilized by intermolecular N—H...Cl and N—H...O hydrogen bonds, one of which is bifurcated.

  8. CCDC 860713: Experimental Crystal Structure Determination : catena-[dimethylammonium (mu-5,5'-ethyne-1,2-diyldiisophthalato)-indium N,N-dimethylformamide dimethyl sulfoxide solvate monohydrate

    KAUST Repository

    Zheng, Bing; Sun, Xiaodong; Li, Guanghua; Cairns, Amy J.; Kravtsov, Victor Ch.; Huo, Qisheng; Liu, Yunling; Eddaoudi, Mohamed

    2016-01-01

    An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

  9. Experimental and theoretical characterization of organic salt: 2-((4-bromophenyl)amino) pyrido[1,2-a] quinoxalin-11-ium bromide monohydrate synthesized via oxidative cyclization

    Science.gov (United States)

    Faizi, Md. Serajul Haque; Alam, Mohammad Jane; Haque, Ashanul; Ahmad, Shabbir; Shahid, M.; Ahmad, Musheer

    2018-03-01

    Quinoxalines are nitrogen-embedded heterocyclic compounds that possess unique and versatile pharmacological applications. The present article describes synthesis and characterization of organic salt 2-((4-bromophenyl)amino)pyrido [1,2-a]quinoxalin-11-ium bromide (BAPQ), an oxidative cyclized product of N-phenyl-N-(pyridine-2-ylmethylene)benzene-1,4-diamine (PPMD). The structure of the synthesized product was extensively characterized by 1H NMR, 2D-COSY NMR, MS, IR, UV-vis, X-ray techniques and elemental analysis. The electronic and structural properties of BAPQ was well complemented by performing extensive computational studies (B3LYP/6-311G (d,p) basis sets). Metal-free, mild reaction condition, easy work-up and excellent yield with high purity are main features of this work and thus holds promise for the generation of new compounds of this class. Analytical results indicated ionic nature of the compound with bromide as counterion. DFT calculation showed low kinetic stability and high reactivity of the compound.

  10. (S,Z-3-Phenyl-2-[(1,1,1-trichloro-7-methoxy-2,7-dioxohept-3-en-4-ylamino]propanoic acid monohydrate

    Directory of Open Access Journals (Sweden)

    Alex Fabiani Claro Flores

    2014-02-01

    Full Text Available In the title compound, C17H18Cl3NO5·H2O, intramolecular N—H...O and C—H...Cl hydrogen bonds form S(6 and S(5 ring motifs, respectively. The chiral organic molecule is connected to the solvent water molecule by a short O—H...O hydrogen bond. In the crystal, a weak C—H...Cl interaction connects the organic molecules along [100] while the water molecules act as bridges between the organic molecules in both the [100] and [010] directions, generating layers parallel to the ab plane.

  11. Crystal structure of N-[3-(dimethylazaniumylpropyl]-N′,N′,N′′,N′′-tetramethyl-N-(N,N,N′,N′-tetramethylformamidiniumylguanidinium dibromide hydroxide monohydrate

    Directory of Open Access Journals (Sweden)

    Ioannis Tiritiris

    2015-12-01

    Full Text Available The asymmetric unit of the title hydrated salt, C15H37N63+·2Br−·OH−·H2O, contains one cation, three partial-occupancy bromide ions, one hydroxide ion and one water molecule. Refinement of the site-occupancy factors of the three disordered bromide ions converges with occupancies 0.701 (2, 0.831 (2 and 0.456 (2 summing to approximately two bromide ions per formula unit. The structure was refined as a two-component inversion twin with volume fractions 0.109 (8:0.891 (8 for the two domains. The central C3N unit of the bisamidinium ion is linked to the aliphatic propyl chain by a C—N single bond. The other two bonds in this unit have double-bond character as have the four C—N bonds to the outer NMe2 groups. In contrast, the three C—N bonds to the central N atom of the (dimethylazaniumylpropyl group have single-bond character. Delocalization of the two positive charges occurs in the N/C/N and C/N/C planes, while the third positive charge is localized on the dimethylammonium group. The crystal structure is stabilized by O—H...O, N—H...Br, O—H...Br and C—H...Br hydrogen bonds, forming a three-dimensional network.

  12. 3,3´-(Ethane-1,2-diyl)bis(6-methoxy-3,4-dihydro-2H-1,3- benzoxazine) monohydrate

    Czech Academy of Sciences Publication Activity Database

    Rivera, A.; Camacho, J.; Ríos-Motta, J.; Kučeráková, Monika; Dušek, Michal

    2012-01-01

    Roč. 68, Part 9 (2012), "o2734"-"sup5" ISSN 1600-5368 Grant - others:AV ČR(CZ) AP0701 Program:Akademická prémie - Praemium Academiae Institutional research plan: CEZ:AV0Z10100521 Keywords : single-crystal X-ray study * T = 120 K * mean δ(C–C) = 0.002 * R factor = 0.030 * wR factor = 0.94 * data-to-parameter ratio = 12.9 Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.347, year: 2011

  13. Crystal structure of 2-amino-4-methyl-pyridin-1-ium (2R,3R)-3-carb-oxy-2,3-di-hydroxy-propano-ate monohydrate.

    Science.gov (United States)

    Jovita, J V; Sathya, S; Usha, G; Vasanthi, R; Ramanand, A

    2014-09-01

    The title mol-ecular salt, C6H9N2 (+)·C4H5O6 (-)·H2O, crystallized with two 2-amino-4-methyl-pyridin-1-ium cations, two l-(+)-tartaric acid monoanions [systematic name: (2R,3R)-3-carb-oxy-2,3-di-hydroxy-propano-ate] and two water mol-ecules in the asymmetric unit. In the crystal, the cations, anions and water mol-ecules are linked via a number of O-H⋯O and N-H⋯O hydrogen bonds, and a C-H⋯O hydrogen bond, forming a three-dimensional structure.

  14. Tris[(6S)-6-hy-droxy-4-epi-shikimic acid] monohydrate: an enanti-omerically pure hy-droxy-lated shikimic acid derived from methyl shikimate.

    Science.gov (United States)

    Griesbeck, Axel G; Miara, Claus; Neudörfl, Jörg-M

    2012-11-01

    The title compound, 3C(7)H(10)O(6)·H(2)O, is the enanti-omerically pure product of a multi-step synthesis from the enanti-omerically pure natural shikimic acid. The asymmetric unit contains three mol-ecules of the acid and one mol-ecule of water. The cyclo-hexene rings of the acids have half-chair conformations. The carboxyl-ate, the four hydroxide groups and the additional water mol-ecule form a complex three-dimensional hydrogen-bonding network.

  15. Crystal structures of diaquadi-μ-hydroxido-tris[trimethyltin(IV] diformatotrimethylstannate(IV and di-μ-hydroxido-tris[trimethyltin(IV] chloride monohydrate

    Directory of Open Access Journals (Sweden)

    Felix Otte

    2016-10-01

    Full Text Available The title compounds, [Sn3(CH39(OH2(H2O2][Sn(CH33(CHO22] (1 and [Sn3(CH39(OH2]Cl·H2O (2, are partially condensed products of hydrolysed trimethyltin chloride. In the structures of 1 and 2, short cationic tristannatoxanes (C9H29O2Sn3 are bridged by a diformatotrimethyltin anion or a chloride anion, respectively. Hydrogen bridges are present and supposedly stabilize these structures against further polymerization to the known polymeric trimethyltin hydroxide. Especially noteworthy is that the formate present in this structure was formed from atmospheric CO2.

  16. 2,4,6-Tri-amino-1,3,5-triazin-1-ium 3-(prop-2-eno-yloxy)propano-ate acrylic acid monosolvate monohydrate.

    Science.gov (United States)

    Sangeetha, V; Kanagathara, N; Chakkaravarthi, G; Marchewka, M K; Anbalagan, G

    2013-05-01

    The asymmetric unit of the title salt, C3H7N6 (+)·C6H7O4 (-)·C3H4O2·H2O, contains a 2,4,6-tri-amino-1,3,5-triazin-1-ium cation, a 3-(prop-2-eno-yloxy)propano-ate anion and acrylic acid and water solvent mol-ecules in a 1:1:1:1 ratio and with each species in a general position. In the crystal, the components are linked into a supra-molecular layer in the bc plane via a combination of O-H⋯O, N-H⋯N and N-H⋯O hydrogen bonding. The crystal studied was a non-merohedral twin, the minor component contribution being approximately 26%.

  17. Creatine Monohydrate Supplementation Does Not Augment Fitness, Performance, or Body Composition Adaptations in Response to Four Weeks of High-Intensity Interval Training in Young Females.

    Science.gov (United States)

    Forbes, Scott C; Sletten, Nathan; Durrer, Cody; Myette-Côté, Étienne; Candow, D; Little, Jonathan P

    2017-06-01

    High-intensity interval training (HIIT) has been shown to improve cardiorespiratory fitness, performance, body composition, and insulin sensitivity. Creatine (Cr) supplementation may augment responses to HIIT, leading to even greater physiological adaptations. The purpose of this study was to determine the effects of 4 weeks of HIIT (three sessions/week) combined with Cr supplementation in recreationally active females. Seventeen females (age = 23 ± 4 yrs; BMI = 23.4 ± 2.4) were randomly assigned to either Cr (Cr; 0.3 g・kg -1 ・d -1 for 5 d followed by 0.1 g・kg -1 ・d -1 for 23 days; n = 9) or placebo (PLA; n = 8). Before and after the intervention, VO 2peak , ventilatory threshold (VT), time-trial performance, lean body mass and fat mass, and insulin sensitivity were assessed. HIIT improved VO 2peak (Cr = +10.2%; PLA = +8.8%), VT (Cr = +12.7%; PLA = +9.9%), and time-trial performance (Cr = -11.5%; PLA = -11.6%) with no differences between groups (time main effects, all p body lean mass (Cr = +0.5%; PLA = -0.9%), or insulin resistance (Cr = +3.9%; PLA = +18.7%). In conclusion, HIIT is an effective way to improve cardiorespiratory fitness, VT, and time-trial performance. The addition of Cr to HIIT did not augment improvements in cardiorespiratory fitness, performance or body composition in recreationally active females.

  18. N-[5-Methyl-2-(2-nitro-phen-yl)-4-oxo-1,3-thia-zolidin-3-yl]pyridine-3-carboxamide monohydrate.

    Science.gov (United States)

    Akkurt, Mehmet; Celik, Ismail; Demir, Hale; Ozkırımlı, Sumru; Büyükgüngör, Orhan

    2011-01-08

    In the title compound, C(16)H(14)N(4)O(4)S·H(2)O, the benzene and pyridine rings make a dihedral angle of 85.8 (1)°. Both enanti-omers of the chiral title compound are statistically disordered over the same position in the unit cell. The methyl and carbonyl group attached to the stereogenic center (C(5) of the thia-zolidine ring) were therefore refined with common site-occupation factors of 0.531 (9) and 0.469 (9), respectively, for each stereoisomer. In the crystal, inter-molecular N-H⋯O, O-H⋯O and O-H⋯N hydrogen bonds link the mol-ecules, forming a three-dimensional supra-molecular network. The crystal structure further shows π-π stacking inter-actions [centroid-centroid distance = 3.5063 (13) Å] between the pyridine rings.

  19. Drug: D02120 [KEGG MEDICUS

    Lifescience Database Archive (English)

    Full Text Available D02120 Mixture ... Drug Citric acid monohydrate - potassium bicarbonate mixt; K-lyte... (TN) Citric acid monohydrate [DR:D01222], Potassium bicarbonate [DR:D02077] ... PubChem: 7849181 LigandBox: D02120 ...

  20. Migrating hydrogen in 2,4,6-triaminopyrimidinium(1+).sub.x./sub. hydrogen trioxofluorophosphate(1-).sub.x./sub. monohydrate/2,4,6-triaminopyrimidinium(2+).sub.1–x./sub.trioxofluorophosphate(2–).sub.1–x./sub. monohydrate(0.0 < x < 0.73) with changing temperature

    Czech Academy of Sciences Publication Activity Database

    Matulková, I.; Fábry, Jan; Němec, I.; Císařová, I.; Vaněk, Přemysl

    2017-01-01

    Roč. 73, Jun (2017), s. 1114-1124 ISSN 2052-5206 Institutional support: RVO:68378271 Keywords : X-ray single-structure determination * hydrogen bonding * pi-pi-electron ring interactions * crystallographic databases * fluorine Subject RIV: BM - Solid Matter Physics ; Magnetism OBOR OECD: Condensed matter physics (including formerly solid state physics, supercond.) Impact factor: 2.032, year: 2016

  1. Poly[[diaqua-μ4-pyrazine-2,3-dicarboxylato-κ6N,O2:O2′:O3,O3′:O3-strontium(II] monohydrate

    Directory of Open Access Journals (Sweden)

    Vahid Amani

    2008-07-01

    Full Text Available In the title compound, {[Sr(C6H2N2O4(H2O2]·H2O}n, the SrII ions are bridged by the pyrazine-2,3-dicarboxylate ligands with the formation of two-dimensional polymeric layers parallel to the ac plane. Each SrII ion is eight-coordinated by one N and five O atoms from the four ligands and two water molecules. The coordination polyhedron is derived from a pentagonal bipyramid with an O atom at the apex on one side of the equatorial plane and two O atoms sharing the apical site on the other side. The coordinated and uncoordinated water molecules are involved in O—H...O and O—H...N hydrogen bonds, which consolidate the crystal structure.

  2. Poly[[tetraaqua(μ3-naphthalene-1,6-disulfonato-κ4O1:O6,O6′:O6′′strontium(II] monohydrate

    Directory of Open Access Journals (Sweden)

    Shan Gao

    2011-12-01

    Full Text Available In the crystal structure of the polymeric title compound, {[Sr(C10H6O6S2(H2O4]·H2O}n, the naphthalene-1,6-disulfonate dianion uses one –SO3 unit to O,O′-chelate to an SrII cation and its third O atom to bind to another SrII cation. The other –SO3 unit binds to yet another SrII atom. The four coordinated water molecules are monodentate but one is disordered over two positions in a 1:1 ratio. The μ3-bonding mode of the dianion generates a polymeric three-dimensional network; the network is consolidated by O—H...O hydrogen bonds. The SrII cation exists in an undefined eight-coordinate environment.

  3. CCDC 1429305: Experimental Crystal Structure Determination : (mu-pyrazole-3,5-dicarboxylato)-(mu-acetato)-bis(2,2':6',2''-terpyridine)-di-ruthenium(ii) chloroform ethanol solvate monohydrate

    KAUST Repository

    Di Giovanni, Carlo; Poater, Albert; Benet-Buchholz, Jordi; Cavallo, Luigi; Sola, Miquel; Llobet, Antoni

    2015-01-01

    An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

  4. (2,2'-Bipyridine-4,4'-dicarboxylic acid-κ2N,N')chlorido(2,2':6',2''-terpyridyl-κ3N,N',N'')ruthenium(II) perchlorate ethanol monosolvate monohydrate

    DEFF Research Database (Denmark)

    Nielsen, Anne; McKenzie, Christine Joy; Bond, Andrew David

    2012-01-01

    ,4 '-dicarboxylic acid ligands, with interplanar separations of 3.65 (1) and 3.72 (1) angstrom. Three O atoms of the perchlorate ion are each disordered equally over two positions. The hydroxy group of the ethanol molecule is also disordered over two sites with refined occupancies of 0.794 (9) and 0.206 (9)....

  5. CCDC 1029959: Experimental Crystal Structure Determination : catena-[tris(triethylammonium) (mu-hydroxo)-bis(mu-1,3,5-benzenetricarboxylato)-bis(mu-5-carboxybenzene-1,3-dicarboxylato)-tetra-cobalt monohydrate

    KAUST Repository

    Lu, Hai-Sheng

    2014-01-01

    An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

  6. Bis(2,2′-bipyridine[1,9-bis(diphenylphosphanyl-1,2,3,4,6,7,8,9-octahydropyrimido[1,2-a]pyrimidin-5-ium]ruthenium(II hexafluoridophosphate dibromide dichloromethane disolvate monohydrate

    Directory of Open Access Journals (Sweden)

    Alain Igau

    2013-12-01

    Full Text Available In the cation of the title complex, [Ru(C31H32N3P2(C10H8N22](PF6(Br2·2CH2Cl2·H2O, the ruthenium ion is coordinated in a distorted octahedral geometry by two 2,2′-bipyridine (bpy ligands and a chelating cationic N-diphenylphosphino-1,3,4,6,7,8-hexahydro-2-pyrimido[1,2-a]pyrimidine [(PPh22-hpp] ligand. The tricationic charge of the complex is balanced by two bromide and one hexafluoridophosphate counter-anions. The compound crystallized with two molecules of dichloromethane (one of which is equally disordered about a Cl atom and a water molecule. In the crystal, one of the Br anions bridges two water molecules via O—H...Br hydrogen bonds, forming a centrosymmetric diamond-shaped R42(8 motif. The cation and anions and the solvent molecules are linked via C—H...F, C—H...Br, C—H...Cl and C—H...O hydrogen bonds, forming a three-dimensional network.

  7. Tris(1,10-phenanthroline-κ2N,N′iron(II bis[(1,10-phenanthroline-κ2N,N′tetrakis(thiocyanato-κNchromate(III] acetonitrile trisolvate monohydrate

    Directory of Open Access Journals (Sweden)

    Volodymyr V. Bon

    2012-05-01

    Full Text Available Single crystals of the title heterometallic compound, [Fe(C12H8N23][Cr(NCS4(C12H8N2]2·3CH3CN·H2O or [Fe(Cphen3][Cr(NCS4(phen]2·3CH3CN·H2O, were prepared using the one-pot open-air reaction of iron powder, Reineckes salt and 1,10-phenanthroline (phen in acetonitrile. The asymetric unit consists of an [Fe(phen3]2+ cation, two [Cr(phen(NCS4]− anions, three acetonitrile solvent molecules and a water molecule. The Fe and Cr atoms both show a slightly distorted octahedral FeN6 and CrN6 coordination geometry with adjacent angles in the range 79.67 (12–95.21 (12°. No classical hydrogen bonding involving the water molecule is observed.

  8. 2-((1E-1-{2-[(2Z-3,4-Diphenyl-2,3-dihydro-1,3-thiazol-2-ylidene]hydrazin-1-ylidene}ethylpyridin-1-ium bromide monohydrate

    Directory of Open Access Journals (Sweden)

    Mehmet Akkurt

    2014-04-01

    Full Text Available In the title compound, C22H19N4S+·Br−·H2O, the dihedral angles between the phenyl groups and the mean plane of the thiazolylidene ring are 34.69 (13 and 64.27 (13°, respectively, while that between the thiazolylidene and pyridinium rings is 14.73 (13°. In the crystal, zigzag chains of alternating bromide ions and water molecules associate through O—H...Br interactions run in channels approximately parallel to the b axis. These chains help form parallel chains of cations through N—H...O, C—H...N and C—H...Br hydrogen bonds.

  9. Crystal structures of 5-amino-N-phenyl-3H-1,2,4-dithiazol-3-iminium chloride and 5-amino-N-(4-chlorophenyl-3H-1,2,4-dithiazol-3-iminium chloride monohydrate

    Directory of Open Access Journals (Sweden)

    Chien Ing Yeo

    2015-10-01

    Full Text Available The crystal and molecular structures of the title salt, C8H8N3S2+·Cl−, (I, and salt hydrate, C8H7ClN3S2+·Cl−·H2O, (II, are described. The heterocyclic ring in (I is statistically planar and forms a dihedral angle of 9.05 (12° with the pendant phenyl ring. The comparable angle in (II is 15.60 (12°, indicating a greater twist in this cation. An evaluation of the bond lengths in the H2N—C—N—C—N sequence of each cation indicates significant delocalization of π-electron density over these atoms. The common feature of the crystal packing in (I and (II is the formation of charge-assisted amino-N—H...Cl− hydrogen bonds, leading to helical chains in (I and zigzag chains in (II. In (I, these are linked by chains mediated by charge-assisted iminium-N+—H...Cl− hydrogen bonds into a three-dimensional architecture. In (II, the chains are linked into a layer by charge-assisted water-O—H...Cl− and water-O—H...O(water hydrogen bonds with charge-assisted iminium-N+—H...O(water hydrogen bonds providing the connections between the layers to generate the three-dimensional packing. In (II, the chloride anion and water molecules are resolved into two proximate sites with the major component being present with a site occupancy factor of 0.9327 (18.

  10. A two-dimensional silver(I) coordination polymer constructed from 4-aminophenylarsonate and triphenylphosphane: poly[[(μ₃-4-aminophenylarsonato-κ³N:O:O)(triphenylphosphane-κP)silver(I)] monohydrate].

    Science.gov (United States)

    Xiao, Zu-Ping; Wen, Meng; Wang, Chun-Ya; Huang, Xi-He

    2015-04-01

    The title compound, {[Ag(C6H7AsNO3)(C18H15P)]·H2O}n, has been synthesized from the reaction of 4-aminophenylarsonic acid with silver nitrate, in aqueous ammonia, with the addition of triphenylphosphane (PPh3). The Ag(I) centre is four-coordinated by one amino N atom, one PPh3 P atom and two arsonate O atoms, forming a severely distorted [AgNPO2] tetrahedron. Two Ag(I)-centred tetrahedra are held together to produce a dinuclear [Ag2O2N2P2] unit by sharing an O-O edge. 4-Aminophenylarsonate (Hapa(-)) adopts a μ3-κ(3)N:O:O-tridentate coordination mode connecting two dinuclear units, resulting in a neutral [Ag(Hapa)(PPh3)]n layer lying parallel to the (101̄) plane. The PPh3 ligands are suspended on both sides of the [Ag(Hapa)(PPh3)]n layer, displaying up and down orientations. There is an R2(2)(8) hydrogen-bonded dimer involving two arsonate groups from two Hapa(-) ligands related by a centre of inversion. Additionally, there are hydrogen-bonding interactions involving the solvent water molecules and the arsonate and amine groups of the Hapa(-) ligands, and weak π-π stacking interactions within the [Ag(Hapa)(PPh3)]n layer. These two-dimensional layers are further assembled by weak van der Waals interactions to form the final architecture.

  11. Crystal structure, vibrational spectra, optical and DFT studies of bis (3-azaniumylpropyl) azanium pentachloroantimonate (III) chloride monohydrate (C6H20N3)SbCl5·Cl·H2O

    Science.gov (United States)

    Ahmed, Houssem Eddine; Kamoun, Slaheddine

    2017-09-01

    The crystal structure of (C6H20N3)SbCl5·Cl·H2O is built up of [NH3(CH2)3NH2(CH2)3NH3]3 + cations, [SbCl5]2 - anions, free Cl- anions and neutral water molecules connected together by Nsbnd H ⋯ Cl, Nsbnd H ⋯ O and Osbnd H ⋯ Cl hydrogen bonds. The optical band gap determined by diffuse reflection spectroscopy (DRS) is 3.78 eV for a direct allowed transition. Optimized molecular geometry, atomic Mulliken charges, harmonic vibrational frequencies, HOMO-LUMO and related molecular properties of the (C6H20N3)SbCl5·Cl·H2O compound were calculated by Density functional theory (DFT) using B3LYP method with GenECP sets. The calculated structural parameters (bond lengths and angles) are in good agreement with the experimental XRD data. The vibrational unscaled wavenumbers were calculated and scaled by a proper scaling factor of 0.984. Acceptable consistency was observed between calculated and experimental results. The assignments of wavenumbers were made on the basis of potential energy distribution (PED) using Vibrational Energy Distribution Analysis (VEDA) software. The HOMO-LUMO study was extended to calculate various molecular parameters like ionization potential, electron affinity, global hardness, electro-chemical potential, electronegativity and global electrophilicity of the given molecule.

  12. Poly[[aqua(μ2-4,4′-bipyridine-κ2N:N′[μ3-3-bromo-2-(carboxylatomethylbenzoato-κ3O1:O1′:O2]cadmium] monohydrate

    Directory of Open Access Journals (Sweden)

    Yangmei Liu

    2012-08-01

    Full Text Available In the title compound, {[Cd(C9H5BrO4(C10H8N2(H2O]·H2O}n, the CdII atom has a distorted octahedral coordination geometry. Two N atoms from two 4,4′-bipyridine (bipy ligands occupy the axial positions, while the equatorial positions are furnished by three carboxylate O atoms from three 3-bromo-2-(carboxylatomethylbenzoate (bcb ligands and one O atom from a water molecule. The bipy and bcb ligands link the CdII atoms into a three-dimensional network. O—H...O hydrogen bonds and π–π interactions between the pyridine and benzene rings [centroid–centroid distance = 3.736 (4 Å] are present in the crystal.

  13. CCDC 1050062: Experimental Crystal Structure Determination : catena-[bis(dimethylammonium) octakis(mu-hydroxo)-tris(mu-1,2,4,5-tetrakis[(4-carboxylato)phenoxymethyl]benzene)-hexaaqua-hexa-yttrium unknown solvate monohydrate

    KAUST Repository

    Luebke, Ryan; Belmabkhout, Youssef; Weseliński, Łukasz J.; Cairns, Amy J.; Alkordi, Mohamed; Norton, George; Wojtas, Łukasz; Adil, Karim; Eddaoudi, Mohamed

    2015-01-01

    An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

  14. CCDC 763927: Experimental Crystal Structure Determination : catena-[tris(mu3-4-Carboxy-2-(pyridin-4-yl)imidazolide-5-carboxylato-N,N1,N3,O,O')-bis(dimethylformamide-O)-tri-zinc dimethylformamide solvate monohydrate

    KAUST Repository

    Jing, Xuemin

    2011-01-01

    An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

  15. Multiple anion . . . π interactions in tris(1,10-phenanthroline-κ.sup.2./sup.N,N’)-iron(II) bis[1,1,3,3-tetracyano-2-(2-hydroxyethyl)propenide] monohydrate

    Czech Academy of Sciences Publication Activity Database

    Zouaoui, S.; Domasevitch, K.V.; Setifi, F.; Mach, P.; Ng, S. W.; Petříček, Václav; Dušek, Michal

    2013-01-01

    Roč. 69, č. 11 (2013), s. 1351-1356 ISSN 0108-2701 Institutional support: RVO:68378271 Keywords : structure analysis, * anion-pi interaction * DFT calculations Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.535, year: 2013

  16. Bis(3,5-di-tert-butyl-4H-1,2,4-triazol-4-amine-κN1(nitrato-κOsilver(I ethanol monosolvate monohydrate

    Directory of Open Access Journals (Sweden)

    Ya-Mei Liu

    2012-06-01

    Full Text Available The AgI atom in the title compound, [Ag(NO3(C10H20N42]·C2H5OH·H2O, is coordinated by the N atoms of two N-heterocycles [N—Ag—N = 151.5 (1°]; the approximately linear coordination geometry is distorted into a T-shaped geometry owing to a long Ag...Onitrate bond [2.717 (4 Å]. The N atoms of the N-heterocycles that are not involved in coordination point towards the lattice water molecule, which functions as a hydrogen-bond donor. The water molecule itself is a hydrogen-bond acceptor towards the ethanol solvent molecule. Hydrogen bonds of the type N–H...O give rise to a layer motif parallel to (001.

  17. Ammonia-water mixtures at high pressures - Melting curves of ammonia dihydrate and ammonia monohydrate and a revised high-pressure phase diagram for the water-rich region. [in primordial solar system ices

    Science.gov (United States)

    Boone, S.; Nicol, M. F.

    1991-01-01

    The phase relations of some mixtures of ammonia and water are investigated to create a phase diagram in pressure-temperature-composition space relevant to the geophysical study of bodies in the outer solar system. The mixtures of NH3(x)H2O(1-x), where x is greater than 0.30 but less than 0.51, are examined at pressures and temperatures ranging from 0-6.5 GPa and 125-400 K, respectively. The ruby luminescence technique monitors the pressure and a diamond-anvil cell compresses the samples, and the phases are identified by means of normal- and polarized-light optical microscopy. The melting curve for NH3H2O(2) is described by the equation T = 176 + 60P - 8.5P squared for the ranges of 0.06-1.4 GPa and 179-243 K. The equation for NH3H2O is T = 194 + 37P - P squared, which represents a minor correction of a previous description by Johnson et al. (1985). Observed phase transitions are consistent with the high-pressure stability limit of NH3H2O(2), and the transition boundary is found to be linear.

  18. Bis[N-(2-aminoethylethane-1,2-diamine-κ3N,N′,N′′]copper(II tris[diamminetetrakis(thiocyanato-κNchromate(III] thiocyanate dimethyl sulfoxide tetradecasolvate monohydrate

    Directory of Open Access Journals (Sweden)

    Vitalina M. Nikitina

    2011-08-01

    Full Text Available The ionic title complex, [Cu(C4H13N32]2[Cr(NCS4(NH32]3(NCS·14C2H6OS·H2O, consists of complex [Cu(dien2]2+ cations [dien is N-(2-aminoethylethane-1,2-diamine], complex [Cr(NCS4(NH32]− anions, an NCS− counter-anion and uncoordinated dimethyl sulfoxide (DMSO and water solvent molecules. One of the Cr atoms lies on an inversion center, while the second Cr atom and the Cu atom lie in general positions. The thiocyanate counter-anion and water molecule are disordered over two positions close to an inversion center. There are several types of hydrogen-bond interactions present in the title compound, which connect the complex cations and anions into bulky [Cu2Cr3] polynuclear species. The four NH3 groups of the complex anions and six bridging DMSO O atoms link the three complex anions via hydrogen bonding into the anionic polynuclear species [Cr(NCS4(NH32]3·6DMSO. The last one is connected by four bridging DMSO O atoms with the two complex copper cations through N—H... O hydrogen bonds between the terminal NH3 groups of the anionic polynuclear species and the NH and NH2 groups of the dien ligand. One additional DMSO molecule is connected via hydrogen bonding to one of the terminal NH3 groups of the anionic polynuclear species. Another DMSO molecule is connected via hydrogen bonding to each Cu(dien2]2+ cation.

  19. Aquachlorido{6,6′-dimethoxy-2,2′-[ethane-1,2-diylbis(nitrilodimethylidyne]diphenolato-κ2O1,N,N′,O1′}cobalt(III monohydrate

    Directory of Open Access Journals (Sweden)

    Jianxin Xing

    2009-04-01

    Full Text Available The title compound, [Co(C18H18N2O4Cl(H2O]·H2O, contains a distorted octahedral cobalt(III complex with a 6,6′-dimethoxy-2,2′-[ethane-1,2-diylbis(nitrilodimethylidyne]diphenolate ligand, a chloride and an aqua ligand, and also a disordered water solvent molecule (half-occupancy. The CoIII ion is coordinated in an N2O3Cl manner. Weak O—H...O hydrogen bonds may help to stabilize the crystal packing.

  20. Diaqua{6,6′-dimethoxy-2,2′-[ethane-1,2-diylbis(nitrilomethylidyne]diphenolato-κ2O,N,N′,O′}manganese(III perchlorate 18-crown-6 hemisolvate monohydrate

    Directory of Open Access Journals (Sweden)

    Ming-Ming Yu

    2009-02-01

    Full Text Available In the cation of the title compound, [Mn(C18H18N2O4(H2O2]ClO4·0.5C12H24O6·H2O, the MnIII ion is coordinated by two water O atoms, and two O atoms and two N atoms from the tetradentate 6,6′-dimethoxy-2,2′-[ethane-1,2-diylbis(nitrilomethylidyne]diphenolate ligand, completing a distorted octahedral geometry. One O atom of the 18-crown-6-ether is disordered over two positions with occupancies of 0.70 (2 and 0.30 (2.

  1. Comparison of Mometasone Furoate Monohydrate (Nasonex and Fluticasone Propionate (Flixonase Nasal Sprays in the Treatment of Dust Mite-sensitive Children with Perennial Allergic Rhinitis

    Directory of Open Access Journals (Sweden)

    Ka-Kit Mak

    2013-08-01

    Conclusion: Following the 4-week therapy, MFM provided greater improvement compared to FP for symptoms of childhood perennial-allergic rhinitis. Based on their TSSs, the MFM group experienced more effective relief of nasal symptoms, whereas the FP group experienced more effective relief of non-nasal symptoms.

  2. Synthesis, crystal structure and magnetic properties of (acetato-κ²O,O')bis(5,5'-dimethyl-2,2'-bipyridine-κ²N,N')nickel(II) perchlorate monohydrate.

    Science.gov (United States)

    Farkašová, Nela; Černák, Juraj; Falvello, Larry R; Orendáč, Martin; Boča, Roman

    2015-04-01

    The title hydrated ionic complex, [Ni(CH3COO)(C12H12N2)2]ClO4·H2O or [Ni(ac)(5,5'-dmbpy)2]ClO4·H2O (where 5,5'-dmbpy is 5,5'-dimethyl-2,2'-bipyridine and ac is acetate), (1), was isolated as violet crystals from the aqueous ethanolic nickel acetate-5,5'-dmbpy-KClO4 system. Within the complex cation, the Ni(II) atom is hexacoordinated by two chelating 5,5'-dmbpy ligands and one chelating ac ligand. The mean Ni-N and Ni-O bond lengths are 2.0628 (17) and 2.1341 (15) Å, respectively. The water solvent molecule is disordered over two partially occupied positions and links two complex cations and two perchlorate anions into hydrogen-bonded centrosymmetric dimers, which are further connected by π-π interactions. The magnetic properties of (1) at low temperatures are governed by the action of single-ion anisotropy, D, which arises from the reduced local symmetry of the cis-NiO2N4 chromophore. The fitting of the variable-temperature magnetic data (2-300 K) gives g(iso) = 2.134 and D/hc = 3.13 cm(-1).

  3. (Acetato-κO(aqua-κO(2-{bis[(3,5-dimethyl-1H-pyrazol-1-yl-κN2methyl]amino-κN}ethanol-κOnickel(II perchlorate monohydrate

    Directory of Open Access Journals (Sweden)

    Jia Zhou

    2012-04-01

    Full Text Available In the structure of the title complex, [Ni(CH3CO2(C14H23N5O(H2O]ClO4·H2O, the NiII centre has a distorted octahedral environment defined by one O and three N atoms derived from the tetradentate ligand, and two O atoms, one from a water molecule and the other from an acetate anion. The molecules are connected into a three-dimensional architecture by O—H...O hydrogen bonds. The perchlorate anion is disordered over two positions; the major component has a site-occupancy factor of 0.525 (19.

  4. (6S,7S,8S,8aS-6-Ethyl-7,8-dihydroxy-1,5,6,7,8,8a-hexahydroindolizin-3(2H-one monohydrate

    Directory of Open Access Journals (Sweden)

    Jozefína Žúžiová

    2010-12-01

    Full Text Available The absolute configuration of the title compound, C10H17NO3·H2O, was assigned from the synthesis. In the molecular structure, the central six-membered ring of the indolizine moiety adopts a chair conformation, with two atoms displaced by −0.578 (2 and 0.651 (1 Å from the plane of the other four atoms [maximum deviation 0.019 (2 Å] The conformation of the fused oxopyrrolidine ring is close to that of a flat envelope, with the flap atom displaced by 0.294 (1 Å from the plane through the remaining four atoms. In the crystal, one of the hydroxy groups is hydrogen-bonded to two water molecules, while the other hydroxy group exhibits an intermolecular hydrogen bond to the carbonyl O atom, resulting in a chain parallel to the b axis.

  5. Crystal structure and spectroscopic analysis of a new oxalate-bridged MnII compound: catena-poly[guanidinium [[aquachloridomanganese(II]-μ2-oxalato-κ4O1,O2:O1′,O2′] monohydrate

    Directory of Open Access Journals (Sweden)

    Hiba Sehimi

    2016-05-01

    Full Text Available As part of our studies on the synthesis and the characterization of oxalate-bridged compounds M–ox–M (ox = oxalate dianion and M = transition metal ion, we report the crystal structure of a new oxalate-bridged MnII phase, {(CH6N3[Mn(C2O4Cl(H2O]·H2O}n. In the compound, a succession of MnII ions (situated on inversion centers adopting a distorted octahedral coordination and bridged by oxalate ligands forms parallel zigzag chains running along the c axis. These chains are interconnected through O—H...O hydrogen-bonding interactions to form anionic layers parallel to (010. Individual layers are held together via strong hydrogen bonds involving the guanidinium cations (N—H...O and N—H...Cl and the disordered non-coordinating water molecule (O—H...O and O—H...Cl, as well as by guanidinium π–π stacking. The structural data were confirmed by IR and UV–Visible spectroscopic analysis.

  6. Crystal structures of fac-trichloridotris(trimethylphosphane-κPrhodium(III monohydrate and fac-trichloridotris(trimethylphosphane-κPrhodium(III methanol hemisolvate: rhodium structures that are isotypic with their iridium analogs

    Directory of Open Access Journals (Sweden)

    Joseph S. Merola

    2015-02-01

    Full Text Available The crystal structures of two solvates of fac-trichloridotris(trimethylphosphane-κPrhodium(III are reported, i.e. one with water in the crystal lattice, fac-[RhCl3(Me3P3]·H2O, and one with methanol in the crystal lattice, fac-[RhCl3(Me3P3]·0.5CH3OH. These rhodium compounds exhibit distorted octahedral coordination spheres at the metal and are isotypic with the analogous iridium compounds previously reported by us [Merola et al. (2013. Polyhedron, 54, 67–73]. Comparison is made between the rhodium and iridium compounds, highlighting their isostructural relationships.

  7. Crystal structures of fac-tri?chlorido?tris?(tri?methyl?phosphane-?P)rhodium(III) monohydrate and fac-tri?chlorido?tris?(tri?methyl?phosphane-?P)rhodium(III) methanol hemisolvate: rhodium structures that are isotypic with their iridium analogs

    OpenAIRE

    Merola, Joseph S.; Franks, Marion A.

    2015-01-01

    The crystal structures of two solvates of fac-tri-chlorido-tris-(tri-methyl-phosphane-κP)rhodium(III) are reported, i.e. one with water in the crystal lattice, fac-[RhCl3(Me3P)3]·H2O, and one with methanol in the crystal lattice, fac-[RhCl3(Me3P)3]·0.5CH3OH. These rhodium compounds exhibit distorted octahedral coordination spheres at the metal and are isotypic with the analogous iridium compounds previously reported by us [Merola et al. (2013 ▶). Polyhedron, 54, 67-73]. Comparison is made bet...

  8. Tris[(6S)-6-hy­droxy-4-epi-shikimic acid] monohydrate: an enanti­omerically pure hy­droxy­lated shikimic acid derived from methyl shikimate

    Science.gov (United States)

    Griesbeck, Axel G.; Miara, Claus; Neudörfl, Jörg-M.

    2012-01-01

    The title compound, 3C7H10O6·H2O, is the enanti­omerically pure product of a multi-step synthesis from the enanti­omerically pure natural shikimic acid. The asymmetric unit contains three mol­ecules of the acid and one mol­ecule of water. The cyclo­hexene rings of the acids have half-chair conformations. The carboxyl­ate, the four hydroxide groups and the additional water mol­ecule form a complex three-dimensional hydrogen-bonding network. PMID:23284468

  9. 2,4,6-Tri­amino-1,3,5-triazin-1-ium 3-(prop-2-eno­yloxy)propano­ate acrylic acid monosolvate monohydrate

    Science.gov (United States)

    Sangeetha, V.; Kanagathara, N.; Chakkaravarthi, G.; Marchewka, M. K.; Anbalagan, G.

    2013-01-01

    The asymmetric unit of the title salt, C3H7N6 +·C6H7O4 −·C3H4O2·H2O, contains a 2,4,6-tri­amino-1,3,5-triazin-1-ium cation, a 3-(prop-2-eno­yloxy)propano­ate anion and acrylic acid and water solvent mol­ecules in a 1:1:1:1 ratio and with each species in a general position. In the crystal, the components are linked into a supra­molecular layer in the bc plane via a combination of O—H⋯O, N—H⋯N and N—H⋯O hydrogen bonding. The crystal studied was a non-merohedral twin, the minor component contribution being approximately 26%. PMID:23723892

  10. Multiple anion...π interactions in tris(1,10-phenanthroline-κ(2)N,N')iron(II) bis[1,1,3,3-tetracyano-2-(2-hydroxyethyl)propenide] monohydrate.

    Science.gov (United States)

    Setifi, Zouaoui; Domasevitch, Konstantin V; Setifi, Fatima; Mach, Pavel; Ng, Seik Weng; Petříček, Vaclav; Dušek, Michal

    2013-11-01

    In the ionic structure of the title compound, [Fe(C12H8N2)3](C9H5N4O2)2·H2O, the octahedral tris-chelate [Fe(phen)3](2+) dications [Fe-N = 1.9647 (14)-1.9769 (14) Å; phen is 1,10-phenathroline] afford one-dimensional chains by a series of slipped π-π stacking interactions [centroid-to-centroid distances = 3.792 (3) and 3.939 (3) Å]. The 1,1,3,3-tetracyano-2-(2-hydroxyethyl)propenide anions, denoted tcnoetOH(-), reveal an appreciable delocalization of π-electron density, involving the central propenide [C-C = 1.383 (3)-1.401 (2) Å] fragment and four nitrile groups, and this is also supported by density functional theory (DFT) calculations at the B97D/6-311+G(2d,2p) level. Primary noncovalent inter-moiety interactions comprise conventional O-H...O(N) and weak C-H...O(N) hydrogen bonding [O...O(N) = 2.833 (2)-3.289 (5) Å and C...O(N) = 3.132 (2)-3.439 (2) Å]. The double anion...π interaction involving a nitrile group of tcnoetOH(-) and two cis-positioned pyridine rings (`π-pocket') of [Fe(phen)3](2+) [N...centroid = 3.212 (2) and 3.418 (2) Å] suggest the relevance of anion...π stackings for charge-diffuse polycyanoanions and common M-chelate species.

  11. 77 FR 74669 - Draft and Revised Draft Guidances for Industry Describing Product-Specific Bioequivalence...

    Science.gov (United States)

    2012-12-17

    ... Phenoxybenzamine hydrochloride Q Quinine sulfate R Risedronate sodium T Tacrolimus Thalidomide Tinidazole For a... Gabapentin P Piroxicam S Sodium Phosphate, dibasic, anhydrous; sodium phosphate, monobasic, monohydrate [[Page 74670

  12. 75 FR 47821 - Endocrinologic and Metabolic Drugs Advisory Committee; Notice of Meeting

    Science.gov (United States)

    2010-08-09

    ... the Sibutramine Cardiovascular Outcomes Trial (SCOUT) (M01- 392), for new drug application (NDA) 20-632, MERIDIA (sibutramine hydrochloride monohydrate) Capsules, sponsored by Abbott Laboratories, for...

  13. 40 CFR 180.910 - Inert ingredients used pre- and post-harvest; exemptions from the requirement of a tolerance.

    Science.gov (United States)

    2010-07-01

    ... surfactants Sucrose octaacetate Adhesive Sulfite liquors and cooking liquors, spent, oxidized (CAS Reg. No... (hydrated alkali aluminum silicate) Solid diluent, carrier Zinc oxide Coating agent Zinc sulfate (basic and monohydrate) Do. Zinc sulfate (basic and monohydrate) Solid diluent, carrier [69 FR 23117, Apr. 28, 2004...

  14. Validation of the ultraviolet spectrophotometry method for the quality control of ciprofloxacin chlorhydrate in Ciprecu tablets

    International Nuclear Information System (INIS)

    Perez Navarro, Maikel; Rodriguez Hernandez, Yaslenis; Suarez Perez, Yania

    2014-01-01

    Quinolones are a group of antimicrobials of high clinical significance. Ciprofloxacin hydrochloride monohydrate is a second-generation antibacterial fluoroquinolone for treatment of several infections and is marketed as eye drops, injections, capsule and tablets. To develop and to validate an ultraviolet spectrophotometric analytical method to be used in the quality control of ciprofloxacin hydrochloride monohydrate in newly manufactured Ciprecu tablets

  15. X-ray studies on piroxicam modifications

    International Nuclear Information System (INIS)

    Reck, G.; Bannier, G.; Hoehne, E.

    1988-01-01

    The anti-inflammatory drug piroxicam, 4-hydroxy-2-methyl-N-(2-pyridyl)2H-1,2-benzothiazine-3-car-boxamide-1,1-dioxide, crystallizes in three different forms, two anhydrates and one monohydrate. Crystal structure analyses of the monohydrate and one of the anhydrate were carried out by Bordner et al. and Kojic-Prodic et al., respectively. The results of the analysis of the third piroxicam modification and of an independently performed structure determination of the monohydrate are reported. Molecular structures and hydrogen bonding of all modifications are discussed. (author)

  16. Modeling and measurements of solid-liquid and vapor-liquid equilibria of polyols and carbohydrates in aqueous solution

    DEFF Research Database (Denmark)

    Jonsdottir, Svava Osk; Cooke, S.A.; Macedo, E.A.

    2002-01-01

    The solubilities of five saccharides in water have been measured at various temperatures. This includes the monosaccharides xylose and galactose, and the disaccharides maltose monohydrate, cellobiose and trehalose dihydrate. A method that uses interaction energies and interaction parameters...

  17. Tritium-proton exchange on fresh and oxidized lecithin

    International Nuclear Information System (INIS)

    Schreiber, J.

    1978-01-01

    A method for exchange labelling of acid protons in lecithin and for their quantitative determination is described. The suitability of the method is discussed using both lecithin monohydrate and autoxidation products as examples. (author)

  18. Characterization of polymorphic solid-state changes using variable temperature X-ray powder diffraction

    DEFF Research Database (Denmark)

    Karjalainen, Milja; Airaksinen, Sari; Rantanen, Jukka

    2005-01-01

    The aim of this study was to use variable temperature X-ray powder diffraction (VT-XRPD) to understand the solid-state changes in the pharmaceutical materials during heating. The model compounds studied were sulfathiazole, theophylline and nitrofurantoin. This study showed that the polymorph form...... of sulfathiazole SUTHAZ01 was very stable and SUTHAZ02 changed as a function of temperature to SUTHAZ01. Theophylline monohydrate changed via its metastable form to its anhydrous form during heating and nitrofurantoin monohydrate changed via amorphous form to its anhydrous form during heating. The crystallinity...... to the anhydrous form. The average crystallite size of sulfathiazole samples varied only a little during heating. The average crystallite size of both theophylline and nitrofurantoin monohydrate decreased during heating. However, the average crystallite size of nitrofurantoin monohydrate returned back to starting...

  19. 40 CFR 180.930 - Inert ingredients applied to animals; exemptions from the requirement of a tolerance.

    Science.gov (United States)

    2010-07-01

    ... Surfactants; related adjuvants of surfactants Sulfite liquors and cooking liquors, spent, oxidized (CAS Reg... animal tag Zinc sulfate (basic and monohydrate) Water repellant, dessicant, and coating agent [69 FR...

  20. In-vitro Release Study of Carvedilol Phosphate Matrix Tablets ...

    African Journals Online (AJOL)

    decreased while Starch 1500 and lactose monohydrate increased drug release. Drug release mechanism ... case of antihypertensive agents to maintain constant blood levels ... systems because of their low toxicity, pH- independent swelling ...

  1. Antidiabetic activity of water extract of Solanum trilobatum (Linn.) in ...

    African Journals Online (AJOL)

    STORAGESEVER

    2009-10-19

    Solanaceae), a medicinal plant widely used in the traditional Ayurveda and Siddha systems of medicine for the treatment of diabetes mellitus was evaluated in the alloxan monohydrate induced diabetic model. Graded doses of the ...

  2. Antidiabetic activity of water extract of Solanum trilobatum (Linn.) in ...

    African Journals Online (AJOL)

    Solanaceae), a medicinal plant widely used in the traditional Ayurveda and Siddha systems of medicine for the treatment of diabetes mellitus was evaluated in the alloxan monohydrate induced diabetic model. Graded doses of the water extract were ...

  3. In situ measurement of solvent-mediated phase transformations during dissolution testing

    DEFF Research Database (Denmark)

    Aaltonen, Jaakko; Heinänen, Paula; Peltonen, Leena

    2006-01-01

    In this study, solvent-mediated phase transformations of theophylline (TP) and nitrofurantoin (NF) were measured in a channel flow intrinsic dissolution test system. The test set-up comprised simultaneous measurement of drug concentration in the dissolution medium (with UV-Vis spectrophotometry......) and measurement of the solid-state form of the dissolving solid (in situ with Raman spectroscopy). The solid phase transformations were also investigated off-line with scanning electron microscopy. TP anhydrate underwent a transformation to TP monohydrate, and NF anhydrate (form beta) to NF monohydrate (form II......). Transformation of TP anhydrate to TP monohydrate resulted in a clear decrease in the dissolution rate, while the transformation of NF anhydrate (form beta) to NF monohydrate (form II) could not be linked as clearly to changes in the dissolution rate. The transformation of TP was an order of magnitude faster than...

  4. Effects of excipients on hydrate formation in wet masses containing theophylline

    DEFF Research Database (Denmark)

    Airaksinen, Sari; Luukkonen, Pirjo; Jørgensen, Anna

    2003-01-01

    its dissolution rate. The aim of this study was to investigate whether excipients, such as alpha-lactose monohydrate or the highly water absorbing silicified microcrystalline cellulose (SMCC) can influence the hydrate formation of theophylline. In particular, the aim was to study if SMCC offers...... protection against the formation of theophylline monohydrate relative to alpha-lactose monohydrate in wet masses after an overnight equilibration and the stability of final granules during controlled storage. In addition, the aim was to study the use of spectroscopic methods to identify hydrate formation...... in the formulations containing excipients. Off-line evaluation of materials was performed using X-ray powder diffractometry, near infrared and Raman spectroscopy. alpha-Lactose monohydrate with minimal water absorbing potential was not able to prevent but enhanced hydrate formation of theophylline. Even though SMCC...

  5. Bulletin of Materials Science | Indian Academy of Sciences

    Indian Academy of Sciences (India)

    . Mineral oxalate monohydrate and di-hydrate are the main organic constituents of kidney stones. However, mechanisms leading to the formation of mineral oxalate kidney stones are not clearly understood. The effect of some urinary stone ...

  6. Crystal structures of 5-amino-N-phenyl-3H-1,2,4-di-thia-zol-3-iminium chloride and 5-amino-N-(4-chloro-phen-yl)-3H-1,2,4-di-thia-zol-3-iminium chloride monohydrate.

    Science.gov (United States)

    Yeo, Chien Ing; Tan, Yee Seng; Tiekink, Edward R T

    2015-10-01

    The crystal and mol-ecular structures of the title salt, C8H8N3S2 (+)·Cl(-), (I), and salt hydrate, C8H7ClN3S2 (+)·Cl(-)·H2O, (II), are described. The heterocyclic ring in (I) is statistically planar and forms a dihedral angle of 9.05 (12)° with the pendant phenyl ring. The comparable angle in (II) is 15.60 (12)°, indicating a greater twist in this cation. An evaluation of the bond lengths in the H2N-C-N-C-N sequence of each cation indicates significant delocalization of π-electron density over these atoms. The common feature of the crystal packing in (I) and (II) is the formation of charge-assisted amino-N-H⋯Cl(-) hydrogen bonds, leading to helical chains in (I) and zigzag chains in (II). In (I), these are linked by chains mediated by charge-assisted iminium-N(+)-H⋯Cl(-) hydrogen bonds into a three-dimensional architecture. In (II), the chains are linked into a layer by charge-assisted water-O-H⋯Cl(-) and water-O-H⋯O(water) hydrogen bonds with charge-assisted iminium-N(+)-H⋯O(water) hydrogen bonds providing the connections between the layers to generate the three-dimensional packing. In (II), the chloride anion and water mol-ecules are resolved into two proximate sites with the major component being present with a site occupancy factor of 0.9327 (18).

  7. (3aS,7aS-5-[(S-3,3,3-Trifluoro-2-methoxy-2-phenylpropanoyl]-2,3,4,5,6,7-hexahydro-1H-pyrrolo[3,4-c]pyridin-3(2H-one monohydrate

    Directory of Open Access Journals (Sweden)

    Huichun Zhu

    2010-01-01

    Full Text Available rac-Benzyl 3-oxohexahydro-1H-pyrrolo[3,4-c]pyridine-5(6H-carboxylate was separated by chiral chromatography, and one of the enantiomers ([α]22D = +10° was hydrogenated in the presence of Pd/C in methanol, producing octahydro-3H-pyrrolo[3,4-c]pyridin-3-one. The latter was reacted with (2R-3,3,3-trifluoro-2-methoxy-2-phenylpropanoyl chloride [(R-(−-Mosher acid chloride], giving rise to the title compound, C17H19F3N2O3·H2O. The present structure established the absolute configuration of the pyrrolopiperidine fragment based on the known configuration of the (R-Mosher acid chloride. The piperidine ring has a somewhat distorted chair conformation and is cis-fused with the five-membered envelope-shaped ring; the plane of the exocyclic amide bond is approximately orthogonal to the plane of the phenyl ring, making a dihedral angle of 82.31 (3°. The water molecule acts as an acceptor to the proton of the amino group in an N—H...O interaction, and as a double proton donor in O—H...O hydrogen bonds, generating infinite bands along the a axis.

  8. CCDC 836213: Experimental Crystal Structure Determination : (S,S)-2-((1,3-Dimethyl-4,5-diphenylimidazolidin-2-ylidene)amino)-1,3-dimethyl-4,5-diphenyl-4,5-dihydro-1H-imidazol-3-ium chloride ethyl acetate solvate monohydrate

    KAUST Repository

    Ma, Ting; Fu, Xiao; Kee, Choon Wee; Zong, Lili; Pan, Yuanhang; Huang, Kuo-Wei; Tan, Choon-Hong

    2011-01-01

    An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

  9. CCDC 866709: Experimental Crystal Structure Determination : catena-(dodecakis(mu~6~-5'-(1H-tetrazol-5-yl)-1,1':3',1''-terphenyl-4,4''-dicarboxylato)-tetrakis(mu~3~-oxo)-hexatriaconta-aqua-tetracosa-copper nitrate monohydrate)

    KAUST Repository

    Eubank, J.F.

    2013-01-01

    An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

  10. Complexes in the Ni2+-imidazole-RN(CH2COO-)2 systems. The crystal structures of tris(imidazole)iminodiacetatonickel(II) monohydrate, hexa(imidazole)nickel(II) bis(N-methyliminodiacetato)nickelate(II) hexahydrate, and tetra(aqua)bis(imidazole)nickel(II) bis(N-benzyliminodiacetato)nickelate(II)

    International Nuclear Information System (INIS)

    Polyakova, I.N.; Sergienko, V.S.; Poznyak, A.L.

    2000-01-01

    Crystals of different compositions, namely, [Ni(Ida)(Im) 3 ] · H 2 O (I), [Ni(Im) 6 ][Ni(Mida) 2 ] · 6H 2 O (II), and [Ni(Im) 2 (H 2 O) 4 ][Ni(Bida) 2 ] (III), have been precipitated from aqueous solutions of the Ni 2+ -Lig 2- Im systems, where Lig 2- is Ida, Mida, and Bida, respectively. The crystal structures of I-III are determined by X-ray diffraction analysis (R = 0.0307, 0.0348, and 0.0302 for 3061, 4706, and 2882 reflections, respectively). Crystals I are built of monomeric mixed-ligand complexes and molecules of crystallization water, which are interlinked by hydrogen bonds into a three-dimensional framework. In II and III, the ligands Lig 2- and Im form charged complexes separately. In II, the cationic and anionic layers of the complexes alternate along the c-axis. Numerous hydrogen bonds involving molecules of crystallization water link the layers into a three-dimensional framework. In III, the cationic and anionic complexes, which serve as proton donors and acceptors, respectively, are bound into layers parallel to the xy plane

  11. CCDC 877424: Experimental Crystal Structure Determination : catena-(Diaqua-(5,10,15,20-tetrakis(N-methylpyridinium-4-yl)porphyrinato)-manganese tetrakis(mu~5~-biphenyl-3,4',5-tricarboxylato)-tetrakis(mu~2~-chloro)-tetrakis(methanol)-hexa-manganese chloride methanol solvate monohydrate)

    KAUST Repository

    Zhang, Zhenjie; Zhang, Linping; Wojtas, L.; Nugent, P.; Eddaoudi, Mohamed; Zaworotko, M.J.

    2012-01-01

    An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

  12. Vertical detachment energies of anionic thymidine: Microhydration effects.

    Science.gov (United States)

    Kim, Sunghwan; Schaefer, Henry F

    2010-10-14

    Density functional theory has been employed to investigate microhydration effects on the vertical detachment energy (VDE) of the thymidine anion by considering the various structures of its monohydrates. Structures were located using a random searching procedure. Among 14 distinct structures of the anionic thymidine monohydrate, the low-energy structures, in general, have the water molecule bound to the thymine base unit. The negative charge developed on the thymine moiety increases the strength of the intermolecular hydrogen bonding between the water and base units. The computed VDE values of the thymidine monohydrate anions are predicted to range from 0.67 to 1.60 eV and the lowest-energy structure has a VDE of 1.32 eV. The VDEs of the monohydrates of the thymidine anion, where the N(1)[Single Bond]H hydrogen of thymine has been replaced by a 2(')-deoxyribose ring, are greater by ∼0.30 eV, compared to those of the monohydrates of the thymine anion. The results of the present study are in excellent agreement with the accompanying experimental results of Bowen and co-workers [J. Chem. Phys. 133, 144304 (2010)].

  13. Analysis of urinary stone based on a spectrum absorption FTIR-ATR

    International Nuclear Information System (INIS)

    Asyana, V; Haryanto, F; Fitri, L A; Ridwan, T; Anwary, F; Soekersi, H

    2016-01-01

    This research analysed the urinary stone by measuring samples using Fourier transform infrared-attenuated total reflection spectroscopy and black box analysis. The main objective of this study is to find kinds of urinary stone and determine a total spectrum, which is a simple model of the chemical and mineral composition urinary stone through black box analysis using convolution method. The measurements result showed that kinds of urinary stone were pure calcium oxalate monohydrate, ion amino acid calcium oxalate monohydrate, a mixture of calcium oxalate monohydrate with calcium phosphate, a mixture of ion amino acid calcium oxalate monohydrate and calcium phosphate,pure uric acid, ion amino acid uric acid, and a mixture of calcium oxalate monohydrate with ion amino acid uric acid. The results of analysis of black box showed characteristics as the most accurate and precise to confirm the type of urinary stones based on theregion absorption peak on a graph, the results of the convolution, and the shape of the total spectrum on each urinary stones. (paper)

  14. Crystal growth and physical characterization of picolinic acid cocrystallized with dicarboxylic acids

    Science.gov (United States)

    Somphon, Weenawan; Haller, Kenneth J.

    2013-01-01

    Pharmaceutical cocrystals are multicomponent materials containing an active pharmaceutical ingredient with another component in well-defined stoichiometry within the same unit cell. Such cocrystals are important in drug design, particularly for improving physicochemical properties such as solubility, bioavailability, or chemical stability. Picolinic acid is an endogenous metabolite of tryptophan and is widely used for neuroprotective, immunological, and anti-proliferative effects within the body. In this paper we present cocrystallization experiments of a series of dicarboxylic acids, oxalic acid, succinic acid, DL-tartaric acid, pimelic acid, and phthalic acid, with picolinic acid. Characterization by FT-IR and Raman spectroscopy, DSC and TG/DTG analysis, and X-ray powder diffraction show that new compounds are formed, including a 1:1 picolinium tartrate monohydrate, a 2:1 monohydrate adduct of picolinic acid and oxalic acid, and a 2:1 picolinic acid-succinic acid monohydrate cocrystal.

  15. Role of excipients in hydrate formation kinetics of theophylline in wet masses studied by near-infrared spectroscopy

    DEFF Research Database (Denmark)

    Jørgensen, Anna C; Airaksinen, Sari; Karjalainen, Milja

    2004-01-01

    . Anhydrous theophylline was chosen as the hydrate-forming model drug compound and two excipients, silicified microcrystalline cellulose (SMCC) and alpha-lactose monohydrate, with different water absorbing properties, were used in formulation. An early stage of wet massing was studied with anhydrous...... theophylline and its 1:1 (w/w) mixtures with alpha-lactose monohydrate and SMCC with 0.1g/g of purified water. The changes in the state of water were monitored using near-infrared spectroscopy, and the conversion of the crystal structure was verified using X-ray powder diffraction (XRPD). SMCC decreased...... the hydrate formation rate by absorbing water, but did not inhibit it. The results suggest that alpha-lactose monohydrate slightly increased the hydrate formation rate in comparison with a mass comprising only anhydrous theophylline....

  16. catena-Poly[[{bis­[tetra­aqua­(2-hy­droxy-3,4-dioxocyclo­but-1-en-1-olato-κO 1)bariumstrontium(0.35/0.65)]di-μ-aqua}­bis­(μ-2-hy­droxy-4-oxocyclo­but-1-ene-1,3-diolato-κ2 O 1:O 3)] monohydrate

    OpenAIRE

    Trifa, Chahrazed; Bouhali, Amira; Bouacida, Sofiane; Boudaren, Chaouki; Bataille, Thierry

    2011-01-01

    International audience; The title structure, {[Ba(0.71)Sr(1.29)(C(4)HO(4))(4)(H(2)O)(10)]*H(2)O}(n), is built from dimers of edge-sharing monocapped square anti-prisms [(Ba/Sr)O(3)(H(2)O)(6)], in which barium and strontium are statistically disordered [ratio 0.353 (8):0.647 (8)] on the same crystallographic site. Such dimers are connected via bidentate hydrogen squarate groups [HC(4)O(4)](-), leading to chains that propagate along the b axis. Inter- and intra-molecular O-H⋯O hydrogen bonds ma...

  17. Renal lithiasis and nutrition

    Directory of Open Access Journals (Sweden)

    Prieto Rafel M

    2006-09-01

    Full Text Available Abstract Renal lithiasis is a multifactorial disease. An important number of etiologic factors can be adequately modified trough diet, since it must be considered that the urine composition is directly related to diet. In fact, the change of inappropriate habitual diet patterns should be the main measure to prevent kidney stones. In this paper, the relation between different dietary factors (liquid intake, pH, calcium, phosphate, oxalate, citrate, phytate, urate and vitamins and each type of renal stone (calcium oxalate monohydrate papillary, calcium oxalate monohydrate unattached, calcium oxalate dihydrate, calcium oxalate dihydrate/hydroxyapatite, hydroxyapatite, struvite infectious, brushite, uric acid, calcium oxalate/uric acid and cystine is discussed.

  18. Validated High Performance Liquid Chromatography Method for ...

    African Journals Online (AJOL)

    Purpose: To develop a simple, rapid and sensitive high performance liquid chromatography (HPLC) method for the determination of cefadroxil monohydrate in human plasma. Methods: Schimadzu HPLC with LC solution software was used with Waters Spherisorb, C18 (5 μm, 150mm × 4.5mm) column. The mobile phase ...

  19. A crystal structure prediction enigma solved

    DEFF Research Database (Denmark)

    Hoser, Anna Agnieszka; Sovago, Ioana; Lanzac, A.

    2017-01-01

    The seemingly unpredictable structure of gallic acid monohydrate form IV has been investigated using accurate X-ray diffraction measurements at temperatures of 10 and 123 K. The measurements demonstrate that the structure is commensurately modulated at 10 K and disordered at higher temperatures...

  20. Contact nuclei formation in aqueous dextrose solutions

    Science.gov (United States)

    Cerreta, Michael K.; Berglund, Kris A.

    1990-06-01

    A laser Raman microprobe was used in situ to observe the growth of alpha dextrose monohydrate on alpha anhydrous dextrose crystals. The Raman spectra indicate growth of the monohydrate below 28.1°C, but the presence of only the anhydrous form above 40.5°C. Contact nucleation experiments with parent anhydrous crystals yielded only monohydrate nuclei below 28.1°C, while contacts in solutions between 34.5 and 41.0°C produced both crystalline forms, and contacts in solutions above 43.5°C produced only anhydrous nuclei. The inability of the monohydrate to grow on anhydrous crystals in the same solution that forms the two crystalline phases with a single contact precludes a simple attrition mechanism of nuclei formation. For the same reason, the hypothetical mechanism involving parent crystal stabilization of pre-crystalline clusters, allowing the clusters to grow into nuclei, is also contradicted. A third, mechanism, which may be a combination of the two, is believed to apply.

  1. Creatine Loading, Resistance Exercise Performance, and Muscle Mechanics.

    Science.gov (United States)

    Stevenson, Scott W.; Dudley, Gary A.

    2001-01-01

    Examined whether creatine (CR) monohydrate loading would alter resistance exercise performance, isometric strength, or in vivo contractile properties of the quadriceps femoris muscle compared with placebo loading in resistance-trained athletes. Overall, CR loading did not provide an ergogenic benefit for the unilateral dynamic knee extension…

  2. Creatine Use and Exercise Heat Tolerance in Dehydrated Men

    OpenAIRE

    Watson, Greig; Casa, Douglas J; Fiala, Kelly A; Hile, Amy; Roti, Melissa W; Healey, Julie C; Armstrong, Lawrence E; Maresh, Carl M

    2006-01-01

    Context: Creatine monohydrate (CrM) use is highly prevalent in team sports (eg, football, lacrosse, ice hockey) and by athletes at the high school, college, professional, and recreational levels. Concerns have been raised about whether creatine use is associated with increased cramping, muscle injury, heat intolerance, and risk of dehydration.

  3. OPTIMIZATION OF TABLET FORMULATIONS BASED ON STARCH LACTOSE GRANULATIONS FOR USE IN TROPICAL COUNTRIES

    NARCIS (Netherlands)

    BOS, CE; BOLHUIS, GK; LERK, CF

    1991-01-01

    Several granulations consisting of alpha-lactose monohydrate 200 mesh and native starch (corn, potato, rice or tapioca) were prepared. The influence of starch concentration, storage temperature and relative humidity on the physical properties of the tablets prepared from these granulations was

  4. Comparative Hypolipidaemic Effects of Allium cepa, Allium sativum ...

    African Journals Online (AJOL)

    Diabetes mellitus was induced in 108 out of a total of 117 adult Rattus novergicus using 150mg/kg b wt of alloxan monohydrate. Increasing dosages (200, 250 and 300mg/kg bw ip) of A. cepa, A. sativum and Z. officinale aqueous extracts were given to the diabetic rats for six weeks while the control rats got either normal ...

  5. THE EFFECT OF DRY GRANULATION ON THE CONSOLIDATION AND COMPACTION OF CRYSTALLINE LACTOSE

    NARCIS (Netherlands)

    RIEPMA, KA; VROMANS, H; ZUURMAN, K; LERK, CF

    1993-01-01

    The consolidation and compaction properties of granule fractions prepared by dry granulation (slugging) of alpha-lactose monohydrate and roller dried beta-lactose, respectively, were studied. The results showed that the compactibility of the granule fractions was determined by the type of lactose

  6. THE RELATIONSHIP BETWEEN BULK-DENSITY AND COMPACTIBILITY OF LACTOSE GRANULATIONS

    NARCIS (Netherlands)

    ZUURMAN, K; RIEPMA, KA; BOLHUIS, GK; VROMANS, H; LERK, CF

    1994-01-01

    The relationship between the bulk density and the compactibility of lactose granulations was studied. The granulations were prepared from different alpha-lactose monohydrate and roller dried beta-lactose powders by wet granulation, using different techniques with only water as a binder, or by

  7. Validated High Performance Liquid Chromatography Method for ...

    African Journals Online (AJOL)

    Purpose: To develop a simple, rapid and sensitive high performance liquid ... response, tailing factor and resolution of six replicate injections was < 3 %. ... Cefadroxil monohydrate, Human plasma, Pharmacokinetics Bioequivalence ... Drug-free plasma was obtained from the local .... Influence of probenicid on the renal.

  8. Subchronic administration of LY354740 does not modify ketamine-evoked behavior and neuronal activity in rats

    NARCIS (Netherlands)

    Imre, Gabor; Fokkema, Dirk S.; Ter Horst, Gert J.

    2006-01-01

    Acute treatment with LY354740 {1S,2S,5R,6S-2-aminobicyclo[3.1.0]hexane-2,6-dicarboxylate monohydrate}, a potent and selective agonist for group 11 metabotropic glutamate receptors (mGlu2/3), has previously been shown to block some schizophrenia-like effects of N-methyl-D-aspartate (NMDA) receptor

  9. Model Compound Studies of Rigid Rod Aromatic Heterocyclic Polymer Systems, the X-Ray Crystal Structure of 2,6-Diphenylbenzo (1,2-d; 5,4-d’) Diimidazole Tetrahydrate, C2OH14N4. 4H2O, a Model System for the Study of Polymer-Water Interaction in Polybenzimidazoles.

    Science.gov (United States)

    1983-07-01

    begin to degrade . The strong affinity for water is manifested by the ability of PBI’s to dry desiccant! Further- more, the observation that crystals of...25. G. M. Brown (1969), "The Crystal Structure of 6- Mercaptopurine Monohydrate," Acta Crystallogr., 3, 210-214. 26. J. Sletten and L. H. Jensen

  10. Synthesis, Characterization and DNA Cleavage of Copper(II ...

    African Journals Online (AJOL)

    Purpose: To study deoxyribonucleic acid (DNA) shearing capability of copper(II) complex of dithiothreitol (DTT) and to fevaluate its potential application in cancer therapy. Methods: A parrot green complex was synthesized by grinding copper acetate monohydrate and DTT in 1:2 molar ratio in a mortar until no fumes of acetic ...

  11. Use of roughness maps in visualisation of surfaces

    DEFF Research Database (Denmark)

    Seitavuopio, Paulus; Rantanen, Jukka; Yliruusi, Jouko

    2005-01-01

    monohydrate, theophylline anhydrate, sodium chloride and potassium chloride. The roughness determinations were made by a laser profilometer. The new matrix method gives detailed roughness maps, which are able to show local variations in surface roughness values and provide an illustrative picture...

  12. Drug: D06100 [KEGG MEDICUS

    Lifescience Database Archive (English)

    Full Text Available D06100 Drug Tezacitabine (USAN); Tezacitabine monohydrate ... C10H12FN3O4. H2O D06100.gif ... Antineoplastic... ... DG01958 ... Nucleic acid derivative, antineoplastic ... DG01439 ... Arabinofuranosyl type antineoplastic... ... DG01439 ... Arabinofuranosyl type antineoplastic Unclassified ... DG02018 ... Antimetabolite ... DG01958 ... Nucleic acid derivative, antineoplastic ... DG01439 ... Arabinofuranosyl type antineoplastic

  13. New gout test: enhanced ex vivo cytokine production from PBMCS in common gout patients and a gout patient with Kearns-Sayre syndrome

    NARCIS (Netherlands)

    Jansen, T.L.; Berendsen, D.; Crisan, T.O.; Cleophas, M.C.; Janssen, M.C.; Joosten, L.A.

    2014-01-01

    Monosodium urate (MSU) monohydrate crystals synergize with various toll-like receptor (TLR) ligands to induce interleukin-(IL)-1beta production. Data are shown from a young male with mitochondriopathy in Kearns-Sayre syndrome (KSS) who developed gout and underwent urate-lowering therapy (ULT) versus

  14. Inorganic salts of biguanide - Searching for new materials for second harmonic generation

    Czech Academy of Sciences Publication Activity Database

    Matulková, Irena; Němec, I.; Císařová, I.; Němec, P.; Mička, Z.

    2008-01-01

    Roč. 886, 1-3 (2008), s. 103-120 ISSN 0022-2860 Institutional research plan: CEZ:AV0Z40400503 Keywords : biguanidium(2+) nitrate * biguanidium(2+) carbonate monohydrate * biguanidium(1+) phosphite trihydrate Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 1.594, year: 2008

  15. In-vitro Release Study of Carvedilol Phosphate Matrix Tablets ...

    African Journals Online (AJOL)

    Microcrystalline cellulose (Avicel PH 101), starch (Sta-Rx 1500) and lactose monohydrate were used as diluents in the formulations while the effect of sodium lauryl sulphate (wetting agent) was studied for some of the formulations. The tablets were characterized for carvedilol phosphate release in both simulated gastric and ...

  16. 21 CFR 558.58 - Amprolium and ethopabate.

    Science.gov (United States)

    2010-04-01

    ... efficiency; as an aid in the prevention of coccidiosis Not for laying chickens; as lincomycin hydrochloride... coccidiosis Not for laying chickens; as lincomycin hydrochloride monohydrate; withdraw 5 d before slaughter... susceptible to chlortetracycline In low calcium feed containing 0.8% dietary calcium and 1.5% sodium sulfate...

  17. Structural basis for the transformation pathways of the sodium naproxen anhydrate-hydrate system

    DEFF Research Database (Denmark)

    Bond, Andrew; Cornett, Claus; Larsen, Flemming Hofmann

    2014-01-01

    to the monohydrate (MH) and anhydrate (AH) structures, provide a basis to rationalize the observed transformation pathways in the sodium (S)-naproxen anhydrate-hydrate system. All structures contain Na(+)/carboxylate/H2O sections, alternating with sections containing the naproxen molecules. The structure of DH...

  18. Studies on tableting properties of lactose. VII. The effect of variations in primary particle size and percentage of amorphous lactose in spray dried lactose products

    NARCIS (Netherlands)

    Vromans, H.; Bolhuis, G.K.; Lerk, C.F.; van de Biggelaar, H.; Bosch, H.

    1987-01-01

    Sieve fractions of α-lactose monohydrate and dicalcium phosphate dihydrate, respectively, suspended in solutions of lactose, were spray dried in order to obtain products with various amorphous lactose contents. The compactibility of the samples appeared to be a function of both the primary particle

  19. CONSOLIDATION AND COMPACTION OF POWDER MIXTURES .1. BINARY-MIXTURES OF SAME PARTICLE-SIZE FRACTIONS OF DIFFERENT TYPES OF CRYSTALLINE LACTOSE

    NARCIS (Netherlands)

    RIEPMA, KA; LERK, CF; DEBOER, AH; BOLHUIS, GK; KUSSENDRAGER, KD

    1990-01-01

    Binary powder mixtures of four different types of crystalline lactose: alpha-lactose monohydrate, anhydrous alpha-lactose, roller-dried beta-lactose and crystalline beta-lactose, were compressed into tablets. The results showed a proportional intercorrelation of the crushing strength and internal

  20. TABLETING PROPERTIES OF EXPERIMENTAL AND COMMERCIALLY AVAILABLE LACTOSE GRANULATIONS FOR DIRECT COMPRESSION

    NARCIS (Netherlands)

    BOLHUIS, GK; ZUURMAN, K

    1995-01-01

    Lactose granulations (125-250 mu m) were prepared from two different alpha-lactose monohydrate powders and one roller dried beta-lactose powder respectively, by wet granulation with only water as a binder. As an effect of the granulation process, the flow properties improved, but the compactibility

  1. Improved Pharmacokinetics of Mercaptopurine Afforded by a Thermally Robust Hemihydrate

    OpenAIRE

    Kersten, Kortney M.; Matzger, Adam J.

    2016-01-01

    Structural and thermal data were obtained for a novel hemihydrate of 6-mercaptopurine. The hemihydrate shows increased solubility and bioavailability when compared to the monohydrate form, better stability against conversion in aqueous media than the anhydrate form, and a dehydration temperature of 240 ?C, the highest of any known hydrate crystal.

  2. Improved pharmacokinetics of mercaptopurine afforded by a thermally robust hemihydrate.

    Science.gov (United States)

    Kersten, Kortney M; Matzger, Adam J

    2016-04-18

    Structural and thermal data were obtained for a novel hemihydrate of 6-mercaptopurine. The hemihydrate shows increased solubility and bioavailability when compared to the monohydrate form, better stability against conversion in aqueous media than the anhydrate form, and a dehydration temperature of 240 °C, the highest of any known hydrate crystal.

  3. Glyoxylate as a reducing agent for manganese(III) in salen scaffold ...

    Indian Academy of Sciences (India)

    being the monohydrate gem-diol forms) followed by the slow electron transfer ... stress and implicated as possible therapeutic agents .... excess HGl at different pHs (1.8–2.5) were set aside ...... sion (UGC), New Delhi in terms of a Teacher Fel-.

  4. randomised double blind study to compare effectiveness of honey

    African Journals Online (AJOL)

    2014-02-02

    Feb 2, 2014 ... EAsT AFRICAN MEDICAL JOURNAL. February 2014 .... based randomised double- blinded clinical trial evaluating effectiveness of ... study drugs was undertaken following a random ... included sodium citrate, citric acid monohydrate, ... post-hoc test to carry out pair-wise comparisons of .... self-care market.

  5. Untitled

    Indian Academy of Sciences (India)

    History effects in low-field magnetoresistance of An electron spin resonance study of Min'" doped. BPSSCO polycrystals 607 calcium hydrazine carboxylate monohydrate. Bainite 131. Some new results in thermomechanical process- Cadmium ing of microalloyed steels 643 Emission spectroscopic determination of B and.

  6. Bulletin of Materials Science | Indian Academy of Sciences

    Indian Academy of Sciences (India)

    Cholesterol (C27H46O) is the most abundant and best-known steroid in the animal kingdom. The in vitro crystallization of this important biomaterial has been attempted by few researchers. Here we are reporting crystallization of pure cholesterol monohydrate crystals in gel medium. It is found that the morphology of the ...

  7. Unusual calcium oxalate crystals in ethylene glycol poisoning.

    Science.gov (United States)

    Godolphin, W; Meagher, E P; Sanders, H D; Frohlich, J

    1980-06-01

    A patient poisoned with ethylene glycol exhibited the symptoms of (1) hysteria, (2) metabolic acidosis with both a large anion gap and osmolal gap, and (3) crystalluria. However, the shape of the urinary crystals was prismatic and resembled hippurate rather than the expected dipyramidal calcium oxalate dihydrate. X-ray crystallography positively identified them as calcium oxalate monohydrate.

  8. THE USE OF A FACTORIAL DESIGN TO EVALUATE THE PHYSICAL STABILITY OF TABLETS PREPARED BY DIRECT COMPRESSION .1. A NEW APPROACH BASED ON THE RELATIVE CHANGE IN TABLET PARAMETERS

    NARCIS (Netherlands)

    Bos, C. E.; BOLHUIS, G. K.; LERK, C. F.; de Boer, J. H.; DUINEVELD, C. A. A.; Smilde, A. K.; Doornbos, D. A.

    1991-01-01

    A factorial design has been used to study the influence of disintegrant concentration and compression force as well as storage temperature and relative humidity on the physical stability during storage of alpha-lactose monohydrate/rice starch tablets prepared by direct compression. The tablet

  9. Growth and characterization of pure and doped NLO L-arginine ...

    Indian Academy of Sciences (India)

    Administrator

    NLO; SHG; solution growth; LAA. 1. Introduction. L-arginine phosphate monohydrate (LAP) was first repor- ted by Xu et al (1983) as a promising nonlinear optical. (NLO) material. LAP is nearly three times more nonlinear than KDP. Monaco et al (1987) reported the formation of. LAP and its chemical analogs from the strongly ...

  10. The investigation of lithium formate hydrate, sodium dithionate and N-methyl taurine as clinical EPR dosimeters

    International Nuclear Information System (INIS)

    Lelie, S.; Hole, E.O.; Duchateau, M.; Schroeyers, W.; Schreurs, S.; Verellen, D.

    2013-01-01

    Introduction: EPR-dosimetry using L-α-alanine is an established method for measuring high doses of ionizing radiation. However, since a minimum dose of approximately 4 Gy is required to achieve sufficient low uncertainties (1–2%) for clinical application, alternative dosimeter materials are being inquired. Lithium formate (LiFo) monohydrate has been studied by several groups and has revealed several promising properties in the low dose region (<4 Gy). The fading properties, however, are somewhat unpredictable, and depend on properties not yet fully uncovered. This paper reports the results from a study of lithium formate hydrate and N-methyl taurine as potential low dose EPR dosimeters. Methods and materials: Pellet shaped dosimeters of lithium formate monohydrate, lithium formate hydrate, sodium dithionate and N-methyl taurine were produced using a manual Weber press, L-α-alanine was obtained from Harwell dosimeters and irradiated using 60 kV and 6 MV X-ray beams, and Co-60 gamma-rays to a dose of 30 Gy and dose ranges of 0.5–100 Gy and 2–20 Gy respectively. The dosimeters were measured using an Electron Paramagnetic Resonance (EPR)-spectrometer. The detector responses for 6 MV and Co-60 radiation beams, the fading behaviors and signal shape in time were investigated. Results: Lithium formate monohydrate and lithium formate hydrate are apparently associated with near identical EPR-spectra (mainly one broad line), and the same spectrum arises for all radiation energies investigated. The shape of the EPR resonance remains constant with time, but the intensities decreases, and the fading is more prominent for the monohydrate than for the hydrate. The EPR resonance associated with N-methyl taurine is more complex than the resonance associated with LiFo and it changes with time, implying radical transitions and growth. Conclusions: The study showed that lithium formate hydrate is a strong candidate for EPR dosimetry with slightly better fading characteristics

  11. A Method for Decreasing the Amount of the Drug Remaining on the Surfaces of the Mortar and Pestle after Grinding Small Amount of Tablets.

    Science.gov (United States)

    Kawakami, Miki; Kitada, Rika; Kurita, Takuro; Tokumura, Tadakazu

    2017-01-01

    The aim of the present study was to develop a method for grinding tablets with a mortar and pestle while reducing drug loss because grinding tablets is known to be associated with reductions in tablet weight and loss of the active drug. Seven kinds of tablets were subjected to grinding. The proportion (%) of the amount of the active drug in the powder remaining on the surfaces of the mortar and pestle relative to the total amount of the drug recovered (the recovery percent) was calculated. The recovery percent of the 7 kinds of tablets ranged from 17.2-35.9%, and the tablets' recovery percent decreased as the tablet weight increased. When the grinding was performed with 1 g of lactose monohydrate or 1 g of D-mannitol moistened with water, the recovery percent of the tablets decreased to 2.6-9.9% and 3.8-9.9%, respectively. The effects of the weight of lactose monohydrate on the recovery percent of Allegra ® 60 mg tablets were examined. It was found that at least 0.6 g of lactose monohydrate was required to have a sufficient effect on drug recovery. Therefore, additives that have stronger effects at lower amounts were sought. As a result, calcium monohydrogen phosphate was found to have the strongest effect on drug recovery. The addition of 0.4 g calcium monohydrogen phosphate resulted in the recovery percent of 5.1%, which was significantly lower than that of 15.0% observed after the addition of 0.4 g lactose monohydrate, and lower than the 6.8% of 1 g lactose monohydrate.

  12. EFSA Panel on Dietetic Products, Nutrition and Allergies (NDA); Scientific Opinion on the substantiation of health claims related to β-hydroxy β-methylbutyrate monohydrate (HMB) alone or in combination with α-ketoisocaproic acid (KIC) and reduction of muscle tissue damage during exercise (ID 1577, , 1584), increase in lean body mass (ID 1579, 1582, 1583), increase in muscle strength (ID 1578, 1583, 1587), increase in endurance performance (ID 1580, 1581), skeletal muscle tissue repair (ID 1586) and faster recovery from muscle fatigue after exercise (ID 1576, 1585) pursuant to Article 13

    DEFF Research Database (Denmark)

    Tetens, Inge

    Following a request from the European Commission, the Panel on Dietetic Products, Nutrition and Allergies was asked to provide a scientific opinion on a list of health claims pursuant to Article 13 of Regulation (EC) No 1924/2006. This opinion addresses the scientific substantiation of health...... and faster recovery from muscle fatigue after exercise. The scientific substantiation is based on the information provided by the Member States in the consolidated list of Article 13 health claims and references that EFSA has received from Member States or directly from stakeholders. The food constituent...

  13. Monitoring of multiple solid-state transformations at tablet surfaces using multi-series near-infrared hyperspectral imaging and multivariate curve resolution

    DEFF Research Database (Denmark)

    Alexandrino, Guilherme L; Khorasani, Milad Rouhi; Amigo Rubio, Jose Manuel

    2015-01-01

    The assessment of the solid-state stability of active pharmaceutical ingredient (API) and/or excipients in solid dosage forms during manufacturing and storage is mandatory for safeguarding quality of the final products. In this work, the solid-state transformations in tablets prepared as blends...... of piroxicam monohydrate (API), polyvinylpyrrolidone and the lactose forms monohydrate or anhydrate were studied when the tablets were exposed to the 23-120°C range. Multi-series near-infrared hyperspectral images were obtained from the surface of each sample for unveiling the local evolution of the solid......-state transformations. The preprocessed spectra from the images (dataset) were arranged in augmented matrices, according to the composition of the tablets, and the profile of the overlapped compounds (relative concentration) along the solid-state transformations in the pixels was resolved by using multivariate curve...

  14. Architecture of the hydrophobic and hydrophilic layers as found from crystal structure analysis of N-benzyl-N,N-dimethylalkylammonium bromides.

    Science.gov (United States)

    Hodorowicz, Maciej; Stadnicka, Katarzyna; Czapkiewicz, Jan

    2005-10-01

    The molecular and crystal structures of N-benzyl-N,N-dimethylalkylammonium bromides monohydrates with chain length n=8-10 have been determined. The crystals are isostructural with the N-benzyl-N,N-dimethyldodecylammonium bromide monohydrate. The structures consist of alternated hydrophobic and hydrophilic layers perpendicular to [001]. The attraction between N+ of the cation head-groups and Br- anions is achieved through weak C_H...Br interactions. The water molecules incorporated into ionic layers are donors for two O_H...Br hydrogen bonds and serve as the acceptors in two weak interactions of C_H...O type. The methylene chains, with the slightly curved general shape, have the extended all-trans conformation. The mutual packing of the chains in the hydrophobic layers is governed by weak C_H...pi interactions.

  15. Formation of a new crystalline form of anhydrous β-maltose by ethanol-mediated crystal transformation.

    Science.gov (United States)

    Verhoeven, Nicolas; Neoh, Tze Loon; Ohashi, Tetsuya; Furuta, Takeshi; Kurozumi, Sayaka; Yoshii, Hidefumi

    2012-04-01

    β-Maltose monohydrate was transformed into an anhydrous form by ethanol-mediated method under several temperatures with agitation. A new stable anhydrous form of β-maltose (Mβ(s)) was obtained, as substantiated by the X-ray diffraction patterns. Mβ(s) obtained by this method presented a fine porous structure, resulting in greater specific surface area compared to those of β-maltose monohydrate and anhydrous β-maltose obtained by vacuum drying (Mβ(h)). The crystal transformation presumably consisted of two steps: dehydration reaction from the hydrous to amorphous forms and crystal formation from the amorphous forms to the noble anhydrous form. The kinetics of these reactions were determined by thermal analysis using Jander's equation and Arrhenius plots. The overall activation energies of the dehydration reaction and the formation of anhydrous maltose were evaluated to be 100 and 90 kJ/mol, respectively. Copyright © 2012 Elsevier Ltd. All rights reserved.

  16. Acute oxalate nephropathy caused by ethylene glycol poisoning

    Directory of Open Access Journals (Sweden)

    Jung Woong Seo

    2012-12-01

    Full Text Available Ethylene glycol (EG is a sweet-tasting, odorless organic solvent found in many agents, such as anti-freeze. EG is composed of four organic acids: glycoaldehyde, glycolic acid, glyoxylic acid and oxalic acid in vivo. These metabolites are cellular toxins that can cause cardio-pulmonary failure, life-threatening metabolic acidosis, central nervous system depression, and kidney injury. Oxalic acid is the end product of EG, which can precipitate to crystals of calcium oxalate monohydrate in the tubular lumen and has been linked to acute kidney injury. We report a case of EG-induced oxalate nephropathy, with the diagnosis confirmed by kidney biopsy, which showed acute tubular injury of the kidneys with extensive intracellular and intraluminal calcium oxalate monohydrate crystal depositions.

  17. Thermal decomposition of lutetium propionate

    DEFF Research Database (Denmark)

    Grivel, Jean-Claude

    2010-01-01

    The thermal decomposition of lutetium(III) propionate monohydrate (Lu(C2H5CO2)3·H2O) in argon was studied by means of thermogravimetry, differential thermal analysis, IR-spectroscopy and X-ray diffraction. Dehydration takes place around 90 °C. It is followed by the decomposition of the anhydrous...... °C. Full conversion to Lu2O3 is achieved at about 1000 °C. Whereas the temperatures and solid reaction products of the first two decomposition steps are similar to those previously reported for the thermal decomposition of lanthanum(III) propionate monohydrate, the final decomposition...... of the oxycarbonate to the rare-earth oxide proceeds in a different way, which is here reminiscent of the thermal decomposition path of Lu(C3H5O2)·2CO(NH2)2·2H2O...

  18. Can a dual-energy computed tomography predict unsuitable stone components for extracorporeal shock wave lithotripsy?

    Science.gov (United States)

    Ahn, Sung Hoon; Oh, Tae Hoon; Seo, Ill Young

    2015-09-01

    To assess the potential of dual-energy computed tomography (DECT) to identify urinary stone components, particularly uric acid and calcium oxalate monohydrate, which are unsuitable for extracorporeal shock wave lithotripsy (ESWL). This clinical study included 246 patients who underwent removal of urinary stones and an analysis of stone components between November 2009 and August 2013. All patients received preoperative DECT using two energy values (80 kVp and 140 kVp). Hounsfield units (HU) were measured and matched to the stone component. Significant differences in HU values were observed between uric acid and nonuric acid stones at the 80 and 140 kVp energy values (penergy values (p<0.001). DECT improved the characterization of urinary stone components and was a useful method for identifying uric acid and calcium oxalate monohydrate stones, which are unsuitable for ESWL.

  19. Calorimetric, FTIR and 1H NMR measurements in combination with DFT calculations for monitoring solid-state changes of dynamics of sibutramine hydrochloride.

    Science.gov (United States)

    Pajzderska, Aleksandra; Chudoba, Dorota M; Mielcarek, Jadwiga; Wąsicki, Jan

    2012-10-01

    Two forms of sibutramine hydrochloride, monohydrate and anhydrous, have been investigated by calorimetric methods, Fourier transform infrared (FTIR) absorption and (1) H nuclear magnetic resonance (NMR) measurements as well as by density functional theory (DFT) of vibrational frequencies and infrared intensities, calculations of steric hindrances and Monte Carlo simulations. The results of FTIR spectra combined with DFT calculations permitted identification of the bands corresponding to the dynamics and vibrations of water molecules. NMR study and Monte Carlo simulations revealed the occurrence of reorientation jumps of the methyl groups in sibutramine cation and also revealed that the reorientation of isopropyl group is possible only in sibutramine monohydrate hydrochloride. The hydration of sibutramine hydrochloride causes a change in the conformation of sibutramine cation. Copyright © 2012 Wiley-Liss, Inc.

  20. Activation of corn cellulose with alcohols to improve its dissolvability in fabricating ultrafine fibers via electrospinning.

    Science.gov (United States)

    Chen, Haizhen; Ni, Jinping; Chen, Jing; Xue, Wenwen; Wang, Jinggang; Na, Haining; Zhu, Jin

    2015-06-05

    Water and four small molecular alcohols are respectively used to activate corn cellulose (CN cellulose) with the aim to improve the dissolvability in DMAc/LiCl. Among all these activated agents, monohydric alcohols are found to produce the optimal effect of activation in the whole process including of activating, dissolving, and electrospinning of CN cellulose. Meanwhile, well distributed fibers with the diameter of 500nm-2μm are fabricated in electrospinning. Understanding the activation effect of monohydric alcohols with water and polyhydric alcohols, the most effective activated agent is ascertained with the characteristics of small molecular size, low viscosity, and single functionality. This work is definitely initiated to understand the critical principle of CN cellulose in dissolving. Accordingly, a feasible methodology is also established to prepare ultrafine cellulose fibers with good morphology in electrospinning. Copyright © 2015 Elsevier Ltd. All rights reserved.

  1. Proton-transfer compounds of 8-hydroxy-7-iodoquinoline-5-sulfonic acid (ferron) with 4-chloroaniline and 4-bromoaniline.

    Science.gov (United States)

    Smith, Graham; Wermuth, Urs D; Healy, Peter C

    2007-07-01

    The crystal structures of the proton-transfer compounds of ferron (8-hydroxy-7-iodoquinoline-5-sulfonic acid) with 4-chloroaniline and 4-bromoaniline, namely 4-chloroanilinium 8-hydroxy-7-iodoquinoline-5-sulfonate monohydrate, C(6)H(7)ClN(+) x C(9)H(5)INO(4)S(-) x H(2)O, and 4-bromoanilinium 8-hydroxy-7-iodoquinoline-5-sulfonate monohydrate, C(6)H(7)BrN(+) x C(9)H(5)INO(4)S(-) x H(2)O, have been determined. The compounds are isomorphous and comprise sheets of hydrogen-bonded cations, anions and water molecules which are extended into a three-dimensional framework structure through centrosymmetric R(2)(2)(10) O-H...N hydrogen-bonded ferron dimer interactions.

  2. Chemical composition and binary mixture of human urinary stones using FT-Raman spectroscopy method.

    Science.gov (United States)

    Selvaraju, R; Raja, A; Thiruppathi, G

    2013-10-01

    In the present study the human urinary stones were observed in their different chemical compositions of calcium oxalate monohydrate, calcium oxalate dihydrate, calcium phosphate, struvite (magnesium ammonium phosphate), uric acid, cystine, oxammite (ammonium oxalate monohydrate), natroxalate (sodium oxalate), glushinkite (magnesium oxalate dihydrate) and moolooite (copper oxalate) were analyzed using Fourier Transform-Raman (FT-Raman) spectroscopy. For the quantitative analysis, various human urinary stone samples are used for ratios calculation of binary mixtures compositions such as COM/COD, HAP/COD, HAP/COD, Uric acid/COM, uric acid/COD and uric acid/HAP. The calibration curve is used for further analysis of binary mixture of human urinary stones. For the binary mixture calculation the various intensities bands at 1462 cm(-1) (I(COM)), 1473 cm(-1) (I(COD)), 961 cm(-1) (I(HAP)) and 1282 cm(-1) (I(UA)) were used. Copyright © 2013 Elsevier B.V. All rights reserved.

  3. 21 CFR 184.1857 - Corn sugar.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Corn sugar. 184.1857 Section 184.1857 Food and... Substances Affirmed as GRAS § 184.1857 Corn sugar. (a) Corn sugar (C6H12O6, CAS Reg. No. 50-99-7), commonly... monohydrate form and is produced by the complete hydrolysis of corn starch with safe and suitable acids or...

  4. Separation of Enantiomers by Preferential Crystallization: Mathematical Modeling of a Coupled Crystallizer Configuration

    DEFF Research Database (Denmark)

    Chaaban, Joussef Hussein; Dam-Johansen, Kim; Skovby, Tommy

    2014-01-01

    A mathematical model describing the separation of enantiomers by simultaneous preferential crystallization in a coupled crystallizer configuration is developed. The model was validated against experimental data for a chemical model compound, the conglomerate forming system of asparagine monohydrate....... The racemic compound and the pure enantiomer can be separated simultaneously in each crystallizer, having sufficient enrichment of the pure enantiomer in the feed solution. The model can also be extended to represent a fully continuous separation process taking into account the continuous supply...

  5. Preparation, Purification and Regioselective Functionalization of Protoescigenin—The Main Aglycone of Escin Complex

    Directory of Open Access Journals (Sweden)

    Krzysztof Woźniak

    2013-04-01

    Full Text Available A two-step chemical process for controlled degradation of escin, affording a mixture of olean-12-ene sapogenins, was elaborated and scaled up. The main component of the mixture—protoescigenin—was isolated and purified, in the form of its corresponding monohydrate, without resource to chromatographic methods. This material was further converted into the high purity 3,24;16,22-di-O,O-isopropylidene derivative in a validated large scale laboratory process.

  6. Cognitive dysfunction in depression - pathophysiology and novel targets

    DEFF Research Database (Denmark)

    Carvalho, Andre F; Miskowiak, Kamilla Woznica; Hyphantis, Thomas N

    2014-01-01

    , inflammation (e.g., enhanced production of pro-inflammatory cytokines), mitochondrial dysfunction, increased apoptosis as well as a diminished neurotrophic support. Several promising neurotherapeutic targets were identified such as minocycline, statins, anti-inflammatory compounds, N-acetylcysteine, omega-3...... poliunsaturated fatty acids, erythropoietin, thiazolidinediones, glucagon-like peptide-1 analogues, S-adenosyl-l-methionine (SAMe), cocoa flavonols, creatine monohydrate and lithium. Erythropoietin and SAMe had pro-cognitive effects in randomized controlled trials (RCT) involving MDD patients. Despite having...

  7. Characterization of crystalline structures in Opuntia ficus-indica

    OpenAIRE

    Contreras-Padilla, Margarita; Rivera-Muñoz, Eric M.; Gutiérrez-Cortez, Elsa; del López, Alicia Real; Rodríguez-García, Mario Enrique

    2014-01-01

    This research studies the crystalline compounds present in nopal (Opuntia ficus-indica) cladodes. The identification of the crystalline structures was performed using X-ray diffraction, scanning electron microscopy, mass spectrometry, and Fourier transform infrared spectroscopy. The crystalline structures identified were calcium carbonate (calcite) [CaCO3], calcium-magnesium bicarbonate [CaMg(CO3)2], magnesium oxide [MgO], calcium oxalate monohydrate [Ca(C2O4)•(H2O)], potassium peroxydiphosph...

  8. ANTI-DIABETIC EFFECTS OF TURMERIC IN ALLOXAN INDUCE D DIABETIC RATS

    OpenAIRE

    Jeevangi; Manjunath; Deepak D; Prakash G; Prashant; Chetan

    2013-01-01

    ABSTRACT: OBJECTIVE AND BACKGROUND: Turmeric (Curcuma longa) is one of the common constituents of our daily food. The present study wa s undertaken to evaluate the anti-diabetic effects of ethanolic extract of Rhizomes of curcuma longa in alloxan induced diabetic rats and compared with of Pioglitazone, which is the standard anti-diabetic agent. METHODS: Alloxan monohydrate is used to induce diabetes mellitus in albino rats in the dose of 120mg/kg i.p. and ...

  9. Thermal decomposition of yttrium(III) propionate and butyrate

    DEFF Research Database (Denmark)

    Grivel, Jean-Claude

    2013-01-01

    The thermal decompositions of yttrium(III) propionate monohydrate (Y(C2H5CO2)3·H2O) and yttrium(III) butyrate dihydrate (Y(C3H7CO2)3·2H2O) were studied in argon by means of thermogravimetry, differential thermal analysis, IR-spectroscopy, X-ray diffraction and hot-stage microscopy. These two...

  10. Electron spin resonance studies of some irradiated pharmaceuticals

    International Nuclear Information System (INIS)

    Gibella, M.; Crucq, A-S.; Tilquin, B.; Stocker, P.; Lesgards, G.; Raffi, J.

    2000-01-01

    Five antibiotics belonging to the cephalosporins and penicillins groups have been irradiated: anhydrous ampicilline acid, amoxicilline acid trihydrate, cefuroxime sodium salt, cloxacilline sodium salt monohydrate and ceftazidime pentahydrate. ESR studies have been carried out, showing the influence of irradiation and storage parameters on the nature and concentration of the free radicals trapped. These results may be used to detect an irradiation treatment on such pharmaceuticals. (author)

  11. Toxicity to rainbow trout of spent still liquors from the distillation of coal

    Energy Technology Data Exchange (ETDEWEB)

    Herbert, D W.M.

    1962-01-01

    From a survey of the literature on the toxicity of ammonium salts, phenol, cyanide, and sulphide to rainbow trout, and from determinations of the toxicity of sodium thiocyanate and sodium thiosulphate, it is postulated that the toxicity of spent still liquors from the distillation of coal should be due mainly to their content of ammonia and monohydric phenols. This is confirmed by experiments showing that the toxicity of an equivalent mixture of ammonium chloride and phenol is nearly as great as that of a spent liquor from a gas works, and that phenol is almost as toxic as mixtures of the monohydric phenols known to be present in such liquors. Experiments on the effect of pH value, hardness, dissolved-oxygen concentration and temperature on the threshold concentration of monohydric phenols are described and compared with similar data for ammonia. Experiments with ammonia and phenols suggest that a mixture of these substances is at its threshold concentration when AS/AT/+PS/PT=I,AS and PS being the concentrations of un-ionized ammonia and monohydric phenols in solution and AT and PT being the threshold concentrations of these substances when tested individually in the same dilution water. A method based on these experiments for predicting the toxicity of ammonia-phenol mixtures from the chemical composition of their solutions is described, and evaluated against laboratory determinations of the toxicity of spent liquors from a coke oven, and against the death or survival of trout held captive in a stream polluted with spent liquor from a gas works. It is concluded that the correspondence between the predicted and observed toxicities is good enough for the method to be used as a basis for assessing whether trout could live in a stream to which a particular spent still liquor was discharged, or when deciding what treatment the effluent should receive to make it safe for such fish after discharge.

  12. INFLUENCE OF CELLULOSE POLYMERIZATION DEGREE AND CRYSTALLINITY ON KINETICS OF CELLULOSE DEGRADATION

    OpenAIRE

    Edita Jasiukaitytė-Grojzdek,; Matjaž Kunaver,; Ida Poljanšek

    2012-01-01

    Cellulose was treated in ethylene glycol with p-toluene sulfonic acid monohydrate as a catalyst at different temperatures. At the highest treatment temperature (150 °C) liquefaction of wood pulp cellulose was achieved and was dependant on cellulose polymerization degree (DP). Furthermore, the rate of amorphous cellulose weight loss was found to increase with cellulose degree of polymerization, while the rate of crystalline cellulose weight loss was reciprocal to the size of the crystallites. ...

  13. Salt forms of the pharmaceutical amide dihydrocarbamazepine.

    Science.gov (United States)

    Buist, Amanda R; Kennedy, Alan R

    2016-02-01

    Carbamazepine (CBZ) is well known as a model active pharmaceutical ingredient used in the study of polymorphism and the generation and comparison of cocrystal forms. The pharmaceutical amide dihydrocarbamazepine (DCBZ) is a less well known material and is largely of interest here as a structural congener of CBZ. Reaction of DCBZ with strong acids results in protonation of the amide functionality at the O atom and gives the salt forms dihydrocarbamazepine hydrochloride {systematic name: [(10,11-dihydro-5H-dibenzo[b,f]azepin-5-yl)(hydroxy)methylidene]azanium chloride, C15H15N2O(+)·Cl(-)}, dihydrocarbamazepine hydrochloride monohydrate {systematic name: [(10,11-dihydro-5H-dibenzo[b,f]azepin-5-yl)(hydroxy)methylidene]azanium chloride monohydrate, C15H15N2O(+)·Cl(-)·H2O} and dihydrocarbamazepine hydrobromide monohydrate {systematic name: [(10,11-dihydro-5H-dibenzo[b,f]azepin-5-yl)(hydroxy)methylidene]azanium bromide monohydrate, C15H15N2O(+)·Br(-)·H2O}. The anhydrous hydrochloride has a structure with two crystallographically independent ion pairs (Z' = 2), wherein both cations adopt syn conformations, whilst the two hydrated species are mutually isostructural and have cations with anti conformations. Compared to neutral dihydrocarbamazepine structures, protonation of the amide group is shown to cause changes to both the molecular (C=O bond lengthening and C-N bond shortening) and the supramolecular structures. The amide-to-amide and dimeric hydrogen-bonding motifs seen for neutral polymorphs and cocrystalline species are replaced here by one-dimensional polymeric constructs with no direct amide-to-amide bonds. The structures are also compared with, and shown to be closely related to, those of the salt forms of the structurally similar pharmaceutical carbamazepine.

  14. Surface area of lactose and lactose granulates on consolidation and compaction

    OpenAIRE

    Riepma, Klaas Alouis

    1993-01-01

    This dissertation discusses the effect of short time storage at different conditions on the strength and the specific BET surface area of lactose tablets. In addition, some aspects are studied of the consolidation and compaction properties of crystalline lactose fractions in heterogeneous systems. The crystalline lactose types used are: a-lactose monohydrate, anhydrous a-lactose, crystalline B-lactose and roller dried B-lactose. ... Zie: Summary

  15. Bulletin of Materials Science | Indian Academy of Sciences

    Indian Academy of Sciences (India)

    ... where MM′ represents MnMn, CoMn, NiMn, CuMn, CoCo, NiCo, CuCo, NiNi, CuNi, and CuCu; and the respective complexes, numbered 1–10, have been prepared by reacting metal(II) salts—i.e. of Mn, Co, Ni, and Cu—and potassium oxalate monohydrate in hot water (90–100°C). The magnetic susceptibility data of the ...

  16. The Regulation and Expression of the Creatine Transporter: A Brief Review of Creatine Supplementation in Humans and Animals

    OpenAIRE

    Schoch, Ryan D; Willoughby, Darryn; Greenwood, Mike

    2006-01-01

    Abstract Creatine monohydrate has become one of the most popular ergogenic sport supplements used today. It is a nonessential dietary compound that is both endogenously synthesized and naturally ingested through diet. Creatine ingested through supplementation has been observed to be absorbed into the muscle exclusively by means of a creatine transporter, CreaT1. The major rationale of creatine supplementation is to maximize the increase within the intracellular pool of total creatine (creatin...

  17. Formation of nitric acid hydrates - A chemical equilibrium approach

    Science.gov (United States)

    Smith, Roland H.

    1990-01-01

    Published data are used to calculate equilibrium constants for reactions of the formation of nitric acid hydrates over the temperature range 190 to 205 K. Standard enthalpies of formation and standard entropies are calculated for the tri- and mono-hydrates. These are shown to be in reasonable agreement with earlier calorimetric measurements. The formation of nitric acid trihydrate in the polar stratosphere is discussed in terms of these equilibrium constants.

  18. A Study of Complexation-ability of Neutral Schiff Bases to Some Metal Cations

    OpenAIRE

    Topal, Giray; Tümerdem, Recep; Basaran, Ismet; Gümüş, Arzu; Cakir, Umit

    2007-01-01

    The constants of the extraction equilibrium and the distribution for dichloromethane as an organic solvent having low dielectric constant of metal cations with chiral Schiff bases, benzaldehydene-(S)-2-amino-3-phenylpropanol (I), ohydroxybenzaldehydene-( S)-2-amino-3-phenyl-propanol (II), benzaldehydene-(S)-2- amino-3-methylbutanol (III) with anionic dyes [4-(2-pyridylazo)-resorcinol mono sodium monohydrate (NaPar), sodium picrat (NaPic) and potassium picrat (KPic)] and some heavy metal chlor...

  19. Electrorheological Properties of Suspensions Prepared from Poly(Li-tert-butyl methacrylate) Ionomer

    OpenAIRE

    YAVUZ, Mustafa

    2014-01-01

    The synthesis, characterisation and partial hydrolysis of poly(tert-butylmethacrylate), (PTBMA), and the electrorheological (ER) properties of its suspensions were investigated. The polymer was synthesised by radical polymerisation and partially hydrolysed by para-toluenesulphonic acid monohydrate (PTSA.H2O), and then converted to a lithium salt (PTBMA-Li) by washing with a LiOH(aq) solution. From particle size measurements, the average particle size of PTBMA-Li was determined to be ...

  20. New Insights into Solid Form Stability and Hydrate Formation: o-Phenanthroline HCl and Neocuproine HCl

    Directory of Open Access Journals (Sweden)

    Doris E. Braun

    2017-12-01

    Full Text Available The moisture- and temperature dependent stabilities and interrelation pathways of the practically relevant solid forms of o-phenanthroline HCl (1 and neocuproine HCl (2 were investigated using thermal analytical techniques (HSM, DSC and TGA and gravimetric moisture sorption/desorption studies. The experimental stability data were correlated with the structural changes observed upon dehydration and the pairwise interaction and lattice energies calculated. For 1 the monohydrate was identified as the only stable form under conditions of RH typically found during production and storage, but at RH values >80% deliquescence occurs. The second compound, 2, forms an anhydrate and two different hydrates, mono- (2-Hy1 and trihydrate (2-Hy3. The 2-Hy1 structure was solved from SCXRD data and the anhydrate structure derived from a combination of PXRD and CSP. Depending on the environmental conditions (moisture either 2-Hy1 or 2-Hy3 is the most sable solid form of 2 at RT. The monohydrates 1-Hy1 and 2-Hy1 show a high enthalpic stabilization (≥20 kJ mol−1 relative to the anhydrates. The anhydrates are unstable at ambient conditions and readily transform to the monohydrates even in the presence of traces of moisture. This study demonstrates how the right combination of experiment and theory can unravel the properties and interconversion pathways of solid forms.

  1. Perspectives on Exertional Rhabdomyolysis.

    Science.gov (United States)

    Rawson, Eric S; Clarkson, Priscilla M; Tarnopolsky, Mark A

    2017-03-01

    Exertional (exercise-induced) rhabdomyolysis is a potentially life threatening condition that has been the subject of research, intense discussion, and media attention. The causes of rhabdomyolysis are numerous and can include direct muscle injury, unaccustomed exercise, ischemia, extreme temperatures, electrolyte abnormalities, endocrinologic conditions, genetic disorders, autoimmune disorders, infections, drugs, toxins, and venoms. The objective of this article is to review the literature on exertional rhabdomyolysis, identify precipitating factors, and examine the role of the dietary supplement creatine monohydrate. PubMed and SPORTDiscus databases were searched using the terms rhabdomyolysis, muscle damage, creatine, creatine supplementation, creatine monohydrate, and phosphocreatine. Additionally, the references of papers identified through this search were examined for relevant studies. A meta-analysis was not performed. Although the prevalence of rhabdomyolysis is low, instances still occur where exercise is improperly prescribed or used as punishment, or incomplete medical history is taken, and exertional rhabdomyolysis occurs. Creatine monohydrate does not appear to be a precipitating factor for exertional rhabdomyolysis. Healthcare professionals should be able to recognize the basic signs of exertional rhabdomyolysis so prompt treatment can be administered. For the risk of rhabdomyolysis to remain low, exercise testing and prescription must be properly conducted based on professional standards.

  2. Direct comparison of low- and mid-frequency Raman spectroscopy for quantitative solid-state pharmaceutical analysis.

    Science.gov (United States)

    Lipiäinen, Tiina; Fraser-Miller, Sara J; Gordon, Keith C; Strachan, Clare J

    2018-02-05

    This study considers the potential of low-frequency (terahertz) Raman spectroscopy in the quantitative analysis of ternary mixtures of solid-state forms. Direct comparison between low-frequency and mid-frequency spectral regions for quantitative analysis of crystal form mixtures, without confounding sampling and instrumental variations, is reported for the first time. Piroxicam was used as a model drug, and the low-frequency spectra of piroxicam forms β, α2 and monohydrate are presented for the first time. These forms show clear spectral differences in both the low- and mid-frequency regions. Both spectral regions provided quantitative models suitable for predicting the mixture compositions using partial least squares regression (PLSR), but the low-frequency data gave better models, based on lower errors of prediction (2.7, 3.1 and 3.2% root-mean-square errors of prediction [RMSEP] values for the β, α2 and monohydrate forms, respectively) than the mid-frequency data (6.3, 5.4 and 4.8%, for the β, α2 and monohydrate forms, respectively). The better performance of low-frequency Raman analysis was attributed to larger spectral differences between the solid-state forms, combined with a higher signal-to-noise ratio. Copyright © 2017 Elsevier B.V. All rights reserved.

  3. Problem of the lithium peroxide thermal stability

    International Nuclear Information System (INIS)

    Nefedov, R A; Ferapontov, Yu A; Kozlova, N P

    2016-01-01

    The behavior of lithium peroxide and lithium peroxide monohydrate samples under heating in atmospheric air was studied by the method of thermogravimetric analysis (TGA) and differential thermal analysis (DTA). It was found that in the temperature range of 32°C to 82°C the interaction of lithium peroxides and steam with the formation of lithium peroxide monohydrate occurs, which was confirmed chemically and by X-ray Single-qualitative analysis. It was experimentally found that lithium peroxide starts to decompose into the lithium oxide and oxygen in the temperature range of 340 ÷ 348°C. It was established that the resulting thermal decomposition of lithium oxide, lithium peroxide at the temperature of 422°C melts with lithium carbonate eutecticly. The manifestation of polymorphism was not marked(seen or noticed) under the heating of studied samples of lithium peroxide and lithium peroxide monohydrate in the temperature range of 25°C ÷ 34°C. (paper)

  4. Sugar-Based Polyamides: Self-Organization in Strong Polar Organic Solvents.

    Science.gov (United States)

    Rosu, Cornelia; Russo, Paul S; Daly, William H; Cueto, Rafael; Pople, John A; Laine, Roger A; Negulescu, Ioan I

    2015-09-14

    Periodic patterns resembling spirals were observed to form spontaneously upon unassisted cooling of d-glucaric acid- and d-galactaric acid-based polyamide solutions in N-methyl-N-morpholine oxide (NMMO) monohydrate. Similar observations were made in d-galactaric acid-based polyamide/ionic liquid (IL) solutions. The morphologies were investigated by optical, polarized light and confocal microscopy assays to reveal pattern details. Differential scanning calorimetry was used to monitor solution thermal behavior. Small- and wide-angle X-ray scattering data reflected the complex and heterogeneous nature of the self-organized patterns. Factors such as concentration and temperature were found to influence spiral dimensions and geometry. The distance between rings followed a first-order exponential decay as a function of polymer concentration. Fourier-Transform Infrared Microspectroscopy analysis of spirals pointed to H-bonding between the solvent and the pendant hydroxyl groups of the glucose units from the polymer backbone. Tests on self-organization into spirals of ketal-protected d-galactaric acid polyamides in NMMO monohydrate confirmed the importance of the monosaccharide's pendant free hydroxyl groups on the formation of these patterns. Rheology performed on d-galactaric-based polyamides at high concentration in NMMO monohydrate solution revealed the optimum conditions necessary to process these materials as fibers by spinning. The self-organization of these sugar-based polyamides mimics certain biological materials.

  5. The phases formed by the dehydration of disodium zirconium (IV) bis(orthophosphate) trihydrate and their ion-exchange behavior

    International Nuclear Information System (INIS)

    Inoue, Yasushi; Yamada, Yoshimune

    1982-01-01

    The phase transformation of Na 2 Zr(PO 4 ) 2 .3H 2 O which had been obtained from zirconium (IV) bis(hydrogenphosphate) monohydrate(α-zirconium phosphate), prepared by the direct precipitation method, was studied by means of gravimetry, X-ray analysis, and acid-base titration. When the material was heated for 2d, it was transformed to a monohydrate at 80 0 C and then successively to three anhydrous phases, depending on the temperature. The monohydrate was also formed by letting the trihydrate stand over P 2 O 5 at room temperature for longer than two weeks. The processes were confirmed to be irreversible by an examination of the rehydration behavior, from which the conditions of the storage of five modifications of disodium zirconium (IV) bis(orthophosphate) were established. It is of special interest that the second anhydrous phase reverted to the first one when it was allowed to stand at room temperature in air or in a desiccator. The rate of the reversion decreased with the temperature of heat-treatment and with a decrease in the relative humidity of the surroundings. The difference between the present results and Clearfield's was clarified and attributed mainly to the difference in the crystallinity of the starting α-zirconium phosphate. (author)

  6. Nondestructive evaluation of crystallized-particle size in lactose-powder by terahertz time-domain spectroscopy

    Science.gov (United States)

    Yamauchi, Satoshi; Hatakeyama, Sakura; Imai, Yoh; Tonouchi, Masayoshi

    2014-03-01

    Transmission-type terahertz time-domain spectroscopy is applied to evaluate crystallized lactose particle of size below 30 μm, which is far too small compared to the wavelength of incident terahertz (THz)-wave. The THz-absorption spectrum of lactose is successfully deconvoluted by Lorentzian to two spectra with peaks at 17.1 cm-1 (0.53 THz) and 45.6 cm-1 (1.37 THz) derived from α-lactose monohydrate, and a spectrum at 39.7 cm-1 (1.19 THz) from anhydrous β-lactose after removal of the broad-band spectrum by polynomial cubic function. Lactose is mainly crystallized into α-lactose monohydrate from the supersaturated solution at room temperature with a small amount of anhydrous β-lactose below 4%. The absorption feature is dependent on the crystallized particle size and the integrated intensity ratio of the two absorptions due to α-lactose monohydrate is correlated in linear for the size.

  7. Origins of hydration differences in homochiral and racemic crystals of aspartic acid.

    Science.gov (United States)

    Juliano, Thomas R; Korter, Timothy M

    2015-02-26

    The propensity for crystalline hydrates of organic molecules to form is related to the strength of the interactions between molecules, including the chiral composition of the molecular solids. Specifically, homochiral versus racemic crystalline samples can exhibit distinct differences in their ability to form energetically stable hydrates. The focus of the current study is a comparison of the crystal structures and intermolecular forces found in solid-state L-aspartic acid, DL-aspartic acid, and L-aspartic acid monohydrate. The absence of experimental evidence for the DL-aspartic acid monohydrate is considered here in terms of the enhanced thermodynamic stability of the DL-aspartic acid anhydrate crystal as compared to the L-aspartic acid anhydrate as revealed through solid-state density functional theory calculations and terahertz spectroscopic measurements. The results indicate that anhydrous DL-aspartic acid is the more stable solid, not due to intermolecular forces alone but also due to the improved conformations of the molecules within the racemic solid. Hemihydrated and monohydrated forms of DL-aspartic acid have been computationally evaluated, and in each case, the hydrates produce destabilized aspartic acid conformations that prevent DL-aspartic acid hydrate formation from occurring.

  8. A paracrine mechanism involving renal tubular cells, adipocytes and macrophages promotes kidney stone formation in a simulated metabolic syndrome environment.

    Science.gov (United States)

    Zuo, Li; Tozawa, Keiichi; Okada, Atsushi; Yasui, Takahiro; Taguchi, Kazumi; Ito, Yasuhiko; Hirose, Yasuhiko; Fujii, Yasuhiro; Niimi, Kazuhiro; Hamamoto, Shuzo; Ando, Ryosuke; Itoh, Yasunori; Zou, Jiangang; Kohri, Kenjiro

    2014-06-01

    We developed an in vitro system composed of renal tubular cells, adipocytes and macrophages to simulate metabolic syndrome conditions. We investigated the molecular communication mechanism of these cells and their involvement in kidney stone formation. Mouse renal tubular cells (M-1) were cocultured with adipocytes (3T3-L1) and/or macrophages (RAW264.7). Calcium oxalate monohydrate crystals were exposed to M-1 cells after 48-hour coculture and the number of calcium oxalate monohydrate crystals adherent to the cells was quantified. The expression of cocultured medium and M-1 cell inflammatory factors was analyzed by enzyme-linked immunosorbent assay and quantitative polymerase chain reaction, respectively. The inflammatory markers MCP-1, OPN and TNF-α were markedly up-regulated in cocultured M-1 cells. OPN expression increased in M-1 cells cocultured with RAW264.7 cells while MCP-1 and TNF-α were over expressed in M-1 cells cocultured with 3T3-L1 cells. Coculturing M-1 cells simultaneously with 3T3-L1 and RAW264.7 cells resulted in a significant increase in calcium oxalate monohydrate crystal adherence to M-1 cells. Inflammatory cytokine changes were induced by coculturing renal tubular cells with adipocytes and/or macrophages without direct contact, indicating that crosstalk between adipocytes/macrophages and renal tubular cells was mediated by soluble factors. The susceptibility to urolithiasis of patients with metabolic syndrome might be due to aggravated inflammation of renal tubular cells triggered by a paracrine mechanism involving these 3 cell types. Copyright © 2014 American Urological Association Education and Research, Inc. Published by Elsevier Inc. All rights reserved.

  9. Laser desorption single-conformation UV and IR spectroscopy of the sulfonamide drug sulfanilamide, the sulfanilamide-water complex, and the sulfanilamide dimer.

    Science.gov (United States)

    Uhlemann, Thomas; Seidel, Sebastian; Müller, Christian W

    2017-06-07

    We have studied the conformational preferences of the sulfonamide drug sulfanilamide, its dimer, and its monohydrated complex through laser desorption single-conformation UV and IR spectroscopy in a molecular beam. Based on potential energy curves for the inversion of the anilinic and the sulfonamide NH 2 groups calculated at DFT level, we suggest that the zero-point level wave function of the sulfanilamide monomer is appreciably delocalized over all four conformer wells. The sulfanilamide dimer, and the monohydrated complex each exhibit a single isomer in the molecular beam. The isomeric structures of the sulfanilamide dimer and the monohydrated sulfanilamide complex were assigned based on their conformer-specific IR spectra in the NH and OH stretch region. Quantum Theory of Atoms in Molecules (QTAIM) analysis of the calculated electron density in the water complex suggests that the water molecule is bound side-on in a hydrogen bonding pocket, donating one O-HO[double bond, length as m-dash]S hydrogen bond and accepting two hydrogen bonds, a NHO and a CHO hydrogen bond. QTAIM analysis of the dimer electron density suggests that the C i symmetry dimer structure exhibits two dominating N-HO[double bond, length as m-dash]S hydrogen bonds, and three weaker types of interactions: two CHO bonds, two CHN bonds, and a chalcogen OO interaction. Most interestingly, the molecular beam dimer structure closely resembles the R dimer unit - the dimer unit with the greatest interaction energy - of the α, γ, and δ crystal polymorphs. Interacting Quantum Atoms analysis provides evidence that the total intermolecular interaction in the dimer is dominated by the short-range exchange-correlation contribution.

  10. The influence of secondary processing on the structural relaxation dynamics of fluticasone propionate.

    Science.gov (United States)

    Depasquale, Roberto; Lee, Sau L; Saluja, Bhawana; Shur, Jagdeep; Price, Robert

    2015-06-01

    This study investigated the structural relaxation of micronized fluticasone propionate (FP) under different lagering conditions and its influence on aerodynamic particle size distribution (APSD) of binary and tertiary carrier-based dry powder inhaler (DPI) formulations. Micronized FP was lagered under low humidity (LH 25 C, 33% RH [relative humidity]), high humidity (HH 25°C, 75% RH) for 30, 60, and 90 days, respectively, and high temperature (HT 60°C, 44% RH) for 14 days. Physicochemical, surface interfacial properties via cohesive-adhesive balance (CAB) measurements and amorphous disorder levels of the FP samples were characterized. Particle size, surface area, and rugosity suggested minimal morphological changes of the lagered FP samples, with the exception of the 90-day HH (HH90) sample. HH90 FP samples appeared to undergo surface reconstruction with a reduction in surface rugosity. LH and HH lagering reduced the levels of amorphous content over 90-day exposure, which influenced the CAB measurements with lactose monohydrate and salmeterol xinafoate (SX). CAB analysis suggested that LH and HH lagering led to different interfacial interactions with lactose monohydrate but an increasing adhesive affinity with SX. HT lagering led to no detectable levels of the amorphous disorder, resulting in an increase in the adhesive interaction with lactose monohydrate. APSD analysis suggested that the fine particle mass of FP and SX was affected by the lagering of the FP. In conclusion, environmental conditions during the lagering of FP may have a profound effect on physicochemical and interfacial properties as well as product performance of binary and tertiary carrier-based DPI formulations.

  11. Binding SnO2 nanocrystals in nitrogen-doped graphene sheets as anode materials for lithium-ion batteries.

    Science.gov (United States)

    Zhou, Xiaosi; Wan, Li-Jun; Guo, Yu-Guo

    2013-04-18

    Hybrid anode materials for Li-ion batteries are fabricated by binding SnO2 nanocrystals (NCs) in nitrogen-doped reduced graphene oxide (N-RGO) sheets by means of an in situ hydrazine monohydrate vapor reduction method. The SnO2NCs in the obtained SnO2NC@N-RGO hybrid material exhibit exceptionally high specific capacity and high rate capability. Bonds formed between graphene and SnO2 nanocrystals limit the aggregation of in situ formed Sn nanoparticles, leading to a stable hybrid anode material with long cycle life. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Stratigraphy and mineralogy of Candor Mensa, West Candor Chasma, Mars: Insights into the geologic history of Valles Marineris

    Science.gov (United States)

    Fueten, F.; Flahaut, J.; Stesky, R.; Hauber, E.; Rossi, A. P.

    2014-02-01

    Candor Mensa, an interior layered deposit (ILD) in Valles Marineris, Mars, consists of two stratigraphically distinct units, the lower of which comprises the bulk of the mensa. This lower unit is approximately 5 km thick and composed of parallel layers, 4 to 14 m in thickness and associated with monohydrated sulfates. The lower unit is disconformably overlain by an upper unit composed of thinner (ancestral basins into the current geometry of Valles Marineris chasmata and that it was possible to form hydrated minerals after this event.

  13. Acute and chronic safety and efficacy of dose dependent creatine nitrate supplementation and exercise performance

    OpenAIRE

    Galvan, Elfego; Walker, Dillon K.; Simbo, Sunday Y.; Dalton, Ryan; Levers, Kyle; O?Connor, Abigail; Goodenough, Chelsea; Barringer, Nicholas D.; Greenwood, Mike; Rasmussen, Christopher; Smith, Stephen B.; Riechman, Steven E.; Fluckey, James D.; Murano, Peter S.; Earnest, Conrad P.

    2016-01-01

    Background Creatine monohydrate (CrM) and nitrate are popular supplements for improving exercise performance; yet have not been investigated in combination. We performed two studies to determine the safety and exercise performance-characteristics of creatine nitrate (CrN) supplementation. Methods Study 1 participants (N?=?13) ingested 1.5?g CrN (CrN-Low), 3?g CrN (CrN-High), 5?g CrM or a placebo in a randomized, crossover study (7d washout) to determine supplement safety (hepatorenal and musc...

  14. Electric field effects in scanning tunneling microscope imaging

    DEFF Research Database (Denmark)

    Stokbro, Kurt; Quaade, Ulrich; Grey, Francois

    1998-01-01

    We present a high-voltage extension of the Tersoff-Hamann theory of scanning tunneling microscope (STM) images, which includes the effect of the electric field between the tip and the sample. The theoretical model is based on first-principles electronic structure calculations and has no adjustable...... parameters. We use the method to calculate theoretical STM images of the monohydrate Si(100)-H(2x1) surface with missing hydrogen defects at -2V and find an enhanced corrugation due to the electric field, in good agreement with experimental images....

  15. Synthesis, characterization and cells and tissues imaging of carbon quantum dots

    Science.gov (United States)

    Wang, Jing; Li, Qilong; Zhou, JingE.; Wang, Yiting; Yu, Lei; Peng, Hui; Zhu, Jianzhong

    2017-10-01

    Compare to other quantum dots, carbon quantum dots have its own incomparable advantages, such as low cell toxicity, favorable biocompatibility, cheap production cost, mild reaction conditions, easy to large-scale synthesis and functionalization. In this thesis, we took citric acid monohydrate and diethylene glycol bis (3-aMinopropyl) ether as materials, used decomposition method to acquire carbon quantum dots (CQDs) which can emission blue fluorescence under ultraviolet excitation. In the aspect of application, we achieved the biological imaging of CQDs in vivo and in vitro.

  16. Internalization of Calcium Oxalate Calculi Developed in Narrow Cavities

    Directory of Open Access Journals (Sweden)

    Fèlix Grases

    2014-03-01

    Full Text Available We describe the case of a patient with calcium oxalate monohydrate and calcium oxalate dihydrate calculi occluded in cavities. All those calculi were located inside narrow cavities covered with a thin epithelium that permits their visualization. Urinary biochemical analysis showed high calciuria, not hypercalciuria, hypocitraturia, and a ratio [calcium]/[citrate] >0.33. The existence of cavities of very low urodynamic efficacy was decisive in the formation of such calculi. It is important to emphasize that we observed a thin epithelium covering such cavities, demonstrating that this epithelium may be formed after the development of the calculi through a re-epithelialization process.

  17. Raman spectra of lithium compounds

    Science.gov (United States)

    Gorelik, V. S.; Bi, Dongxue; Voinov, Y. P.; Vodchits, A. I.; Gorshunov, B. P.; Yurasov, N. I.; Yurasova, I. I.

    2017-11-01

    The paper is devoted to the results of investigating the spontaneous Raman scattering spectra in the lithium compounds crystals in a wide spectral range by the fibre-optic spectroscopy method. We also present the stimulated Raman scattering spectra in the lithium hydroxide and lithium deuteride crystals obtained with the use of powerful laser source. The symmetry properties of the lithium hydroxide, lithium hydroxide monohydrate and lithium deuteride crystals optical modes were analyzed by means of the irreducible representations of the point symmetry groups. We have established the selection rules in the Raman and infrared absorption spectra of LiOH, LiOH·H2O and LiD crystals.

  18. System of ytterbium nitrate-hydrazine(mono-)dinitrate-water

    International Nuclear Information System (INIS)

    Khisaeva, D.A.; Katamanov, V.L.

    1986-01-01

    Solubility in ternary systems ytterbium nitrate-hydrazine monohydrate-water and ytterbium nitrate-hydrazine dinitrate-water is studied at 25 and 50 deg C. Salt components of both systems do not form with each other double addition compounds in the chosen temperature range. Initial salts are equilibrium solid phases of saturated solutions. Correlation of the range of primary crystallization of nitrate acydocomplexes of lanthanides formed in similar systems with their atomic number is considered. It is shown that hydrazine dinitrate can be used for separation of rare earth elements of cerium group

  19. Enzymatic production of alkyl esters through alcoholysis: A critical evaluation of lipases and alcohols

    DEFF Research Database (Denmark)

    Li, Deng; Xu, Xuebing; Gudmundur G, Haraldsson

    2005-01-01

    This paper focuses on a detailed evaluation of commercially available immobilized lipases and simple monohydric alcohols for the production of alkyl esters from sunflower oil by enzymatic alcoholysis. Six lipases were tested with seven alcohols, including straight and branched-chain primary...... in an increased degree of conversion for all lipases except Novozym 435. The secondary alcohol 2-propanol significantly reduced the alcoholysis reaction with all lipases; however, the branch-chain isobutanol was more advantageous than linear 1-butanol for Novozym 435, Lipozyme RM IM, and Lipase PS-C. Many...

  20. Synthese und Charakterisierung wasserfreier Seltenerdmetall-Nitrate, -Acetate und -Oxyacetate

    OpenAIRE

    Heinrichs, Christina

    2013-01-01

    Durch thermische Entwässerung der Seltenerdmetall(SE)-Nitrat-Hydrate und der SE-Acetat-Hydrate im Argon-Strom/Vakuum konnten wasserfreie SE-Nitrate und SE-Nitrat-Monohydrate bzw. wasserfreie SE-Acetate erhalten werden. Es gelang zudem, SE-Oxyacetate durch thermische Zersetzung der SE-Acetate darzustellen. Des Weiteren wurde beim Erhitzen von Praseodym-Carbonat-Hydrat ein Pr-Carbonat-Hydroxid erhalten. Die Verbindungen wurden mittels Röntgenpulverdiffraktometrie und an ausgewählten Beispielen ...

  1. Recurrence rates of urinary calculi according to stone composition and morphology

    DEFF Research Database (Denmark)

    Daudon, Michel; Jungers, Paul; Bazin, Dominique

    2018-01-01

    stone event, with these being more frequent in men (44.4%) than in women (38.9%, p acid (62.5 ± 14.9 years), with the average age of first stones of calcium oxalate falling...... in the middle (40.7 ± 14.6 years for calcium oxalate dihydrate, and 48.4 ± 15.1 years for calcium oxalate monohydrate, COM). By composition alone, COM was among the least recurrent of stones, with only 38.0% of COM stones coming from patients who had had a previous episode; however, when the different...

  2. The LiHCOO-Sc(HCOO)3-H2O system at 25 and 50 deg C

    International Nuclear Information System (INIS)

    Petrova, E.V.; Itkina, L.S.

    1980-01-01

    Solubility in the LiHCOO-Sc(HCOO) 3 -H 2 O system at 25 and 50 deg C has been investigated using the isothermal method It has been ascertainedy s stem is a simple eutonic one. Solubility isotherms consist of two crystallization branches: lithium formate monohydrate and scandium formate. Scandium formate salts-out lithium formate from the solution. Lithium formate increases the solubility of scandium formate (in the eutonic solution more than 2 times as compared to its solubility in the pure water)

  3. Creatine Transporter Deficiency in Two Brothers with Autism Spectrum Disorder.

    Science.gov (United States)

    Aydin, Halil Ibrahim

    2018-01-15

    Creatine transporter deficiency (CTD) is a treatable, X-linked, inborn error of metabolism. Two brothers with autism spectrum disorder were diagnosed with CTD at the ages of 17 and 12 years. Both were found to have a previously reported hemizygous p.408delF (c.1216_1218delTTC) deletion mutation. Both patients were given creatine monohydrate, L-arginine, L-glycine and S-adenosylmethionine, which partially improved the behavioral problems. Serum creatinine levels, creatine peak at brain MR spectroscopy or creatine/creatinine ratio in urine should be evaluated to identify CTD in children with autistic behavior and language disorders.

  4. THE EFFECT OF CREATINE SUPPLEMENTATION ON ATHLETE ISOKINETIC PERFORMANCE

    OpenAIRE

    Erkan Faruk ŞİRİN; Suzan YALÇIN

    2009-01-01

    The purpose of this study is to find the effects of Creatin Monohydrate (CrH2O) on athlete performance (isokinetic power measured as a total workout) used as an ergojenic aid in long-term (6 weeks) supplementation. There are 38 participants willing to join to the study. Their ages are between 20 and 27. All of them are choosed from active athletes. From the findings of this study; all the participants’ in the creatin group have increased the total workout production in all cycles of isokineti...

  5. Increasing alcohol yield in sugar fermentation

    Energy Technology Data Exchange (ETDEWEB)

    Colin, P

    1962-02-20

    The yield of alcohol from yeast fermentations of sugar solutions is increased 1.5 to 5% by the addition of 0.1 to 0.5 parts by volume of a monohydric saturated aliphatic alcohol of at least 6 C atoms in a straight chain such as hexanol or heptanol, or branched chain, such as 2-ethylbutanol or 2-ethylhexanol, or a mixture consisting mostly of C/sub 7/, C/sub 8/, C/sub 9/, or C/sub 10/ alcohols.

  6. (10R,13R-17-(6-Hydroxy-5-methylheptan-2-yl-10,13-dimethyl-2,3,4,7,8,9,10,11,12,13,14,15,16,17-tetradecahydro-1H-cyclopenta[a]phenanthren-3-ol hemihydrate: a bioactive steroid isolated from the Indian herb Artemisia reticulata

    Directory of Open Access Journals (Sweden)

    A. K. Bauri

    2017-08-01

    Full Text Available The title tetracyclic steroidal compound, C27H46O2·0.5H2O, crystallized as a monohydrate with two independent molecules (1 and 2 in the asymmetric unit. In both molecules, the conformations of the three cyclohexane rings (A, B and C are chair, half-chair and chair, respectively. The fourth ring, D, has a twisted conformation on the bond linking the D and C rings. The crystal structure is stabilized by hydrogen bonding with the two independent molecules being linked through the solvent water molecule via various O—H...O hydrogen bonds, forming layers parallel to (-101.

  7. Thermal behavior and decomposition of cerium(III) butanoate, pentanoate and hexanoate salts upon heating in argon

    DEFF Research Database (Denmark)

    Grivel, Jean-Claude; Suarez Guevara, Maria Josefina; Yue, Zhao

    2017-01-01

    The thermal behavior and decomposition of Ce-butanoate monohydrate (Ce(C3H7CO2)3·H2O), Ce-pentanoate (Ce(C4H9CO2)3) and Ce-hexanoate (Ce(C5H11CO2)3) were studied in a flow of argon while heating at 5 °C/min. By means of several techniques such as simultaneous TG-DTA, FTIR evolved gas analysis, in...

  8. Characterization of calcium oxalate biominerals in some (non-Cactaceae) succulent plant species.

    Science.gov (United States)

    Monje, Paula V; Baran, Enrique J

    2010-01-01

    The water-accumulating leaves of crassulacean acid metabolism plants belonging to five different families were investigated for the presence of biominerals by infrared spectroscopic and microscopic analyses. Spectroscopic results revealed that the mineral present in succulent species of Agavaceae, Aizoaceae, and Asphodelaceae was calcium oxalate monohydrate (whewellite, CaC2O4 x H2O). Crystals were predominantly found as raphides or solitary crystals of various morphologies. However, representative Crassulaceae members and a succulent species of Asteraceae did not show the presence of biominerals. Overall, these results suggest no correlation between calcium oxalate generation and crassulacean acid metabolism in succulent plants.

  9. On the structure of amorphous calcium carbonate--a detailed study by solid-state NMR spectroscopy.

    Science.gov (United States)

    Nebel, Holger; Neumann, Markus; Mayer, Christian; Epple, Matthias

    2008-09-01

    The calcium carbonate phases calcite, aragonite, vaterite, monohydrocalcite (calcium carbonate monohydrate), and ikaite (calcium carbonate hexahydrate) were studied by solid-state NMR spectroscopy ( (1)H and (13)C). Further model compounds were sodium hydrogencarbonate, potassium hydrogencarbonate, and calcium hydroxide. With the help of these data, the structure of synthetically prepared additive-free amorphous calcium carbonate (ACC) was analyzed. ACC contains molecular water (as H 2O), a small amount of mobile hydroxide, and no hydrogencarbonate. This supports the concept of ACC as a transient precursor in the formation of calcium carbonate biominerals.

  10. Mechanochemical synthesis and structural characterization of three novel cocrystals of dimethylglyoxime with N-heterocyclic aromatic compounds and acetamide

    Science.gov (United States)

    Abidi, Syed Sibte Asghar; Azim, Yasser; Gupta, Abhishek Kumar; Pradeep, Chullikkattil P.

    2017-12-01

    With an aim to explore the interactions of (RR'Cdbnd Nsbnd OH) oxime moiety of dimethylglyoxime (DMG) with pyridyl ring of N-heterocyclic aromatic compounds and acetamide, three novel cocrystals of dimethylglyoxime with acridine (ACR), 1,10-phenanthroline monohydrate (PT) and acetamide (ACT) are reported. These three cocrystals were obtained with a mechanochemical synthesis approach and were characterized by single crystal X-ray diffraction (SCXRD), powder X-ray diffraction (PXRD), fourier transform-infrared spectroscopy (FT-IR), differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). Additionally, Hirshfeld surface analysis is used to investigate the intermolecular interaction and the crystal packing of cocrystals.

  11. Radiolysis of lignin: Prospective mechanism of high-temperature decomposition

    Science.gov (United States)

    Ponomarev, A. V.

    2017-12-01

    The range of the radiation-thermal processes resulting in conversion of lignin into monomeric phenols is considered. Statistically the most probable places of macromolecule ionization are aromatic units. Release of phenolic products from a lignin macromolecule is the multistage process beginning via fragmentation of primary cation-radicals. Reactions of electrons and small radicals with macromolecules, also as degradation of cation-radicals, result in formation of phenoxyl radicals. Macroradicals possess lower heat stability in comparison with macromolecules. Thermal decomposition of macroradicals leads to release of monohydric and dihydric phenols. The probability of benzenediols formation increases in the presence of alkanes. As noted, partial transformation of lignin into charcoal is inevitable.

  12. Ammonia-water phase diagram and its implications for icy satellites

    International Nuclear Information System (INIS)

    Johnson, M.L.; Nicol, M.

    1986-01-01

    A Holzapfel-type diamond anvil cell is used to determine the NH 3 - H 2 O phase diagram in the region from 0 to 33 mole percent NH 3 , 240 to 370 K, and 0 to 5 GPa. The following phases were identified: liquid; water ices Ih, III, V, VI, VII, and VIII; ammonia monohydrate, NH 3 .H 2 O; and ammonia dihydrate NH 3 . 2 H 2 O. Ammonia dihydrate becomes prominent at moderate pressures (less than 1 GPa), with planetologically significant implications, including the possibility of layering in Titan's magma ocean

  13. Effects of Polyphenols from Grape Seeds on Renal Lithiasis

    Directory of Open Access Journals (Sweden)

    Felix Grases

    2015-01-01

    Full Text Available Nephrolithiasis is a complex disease that results from a combination of factors related to both urine composition and kidney morphoanatomy. Development of calcium oxalate monohydrate papillary calculi is linked to initial subepithelial calcification of renal papilla. Progressive tissue calcification depends on preexisting injury and involves reactive oxygen species. Many plant extracts that protect against oxidative stress manifest antilithiasic activity. Our study focused on determining the effects of polyphenols on a lithiasis rat model. Rats were pretreated with polyphenols and grape seed extracts, followed by posterior induction of hyperoxalosis via treatment with ethylene glycol plus NH4Cl. The concentrations of calcium and other elements in kidney were determined, along with histological examination of kidney and 24 h urine analysis. Significant differences were observed in the renal calcium content between the control plus ethylene glycol-treated group and the epicatechin plus ethylene glycol-treated, red grape seed extract plus ethylene glycol-treated, and white grape seed extract plus ethylene glycol-treated groups, with reductions of about 50%. The antioxidant activity of polyphenols extracted from red and white grape seeds may be critical in the prevention of calcium oxalate monohydrate papillary calculus formation, particularly if calculi are induced by lesions caused by cytotoxic compounds with oxidative capacity.

  14. Aging-driven decomposition in zolpidem hemitartrate hemihydrate and the single-crystal structure of its decomposition products.

    Science.gov (United States)

    Vega, Daniel R; Baggio, Ricardo; Roca, Mariana; Tombari, Dora

    2011-04-01

    The "aging-driven" decomposition of zolpidem hemitartrate hemihydrate (form A) has been followed by X-ray powder diffraction (XRPD), and the crystal and molecular structures of the decomposition products studied by single-crystal methods. The process is very similar to the "thermally driven" one, recently described in the literature for form E (Halasz and Dinnebier. 2010. J Pharm Sci 99(2): 871-874), resulting in a two-phase system: the neutral free base (common to both decomposition processes) and, in the present case, a novel zolpidem tartrate monohydrate, unique to the "aging-driven" decomposition. Our room-temperature single-crystal analysis gives for the free base comparable results as the high-temperature XRPD ones already reported by Halasz and Dinnebier: orthorhombic, Pcba, a = 9.6360(10) Å, b = 18.2690(5) Å, c = 18.4980(11) Å, and V = 3256.4(4) Å(3) . The unreported zolpidem tartrate monohydrate instead crystallizes in monoclinic P21 , which, for comparison purposes, we treated in the nonstandard setting P1121 with a = 20.7582(9) Å, b = 15.2331(5) Å, c = 7.2420(2) Å, γ = 90.826(2)°, and V = 2289.73(14) Å(3) . The structure presents two complete moieties in the asymmetric unit (z = 4, z' = 2). The different phases obtained in both decompositions are readily explained, considering the diverse genesis of both processes. Copyright © 2010 Wiley-Liss, Inc.

  15. Evaluation of Chitosan-Microcrystalline Cellulose Blends as Direct Compression Excipients

    Directory of Open Access Journals (Sweden)

    Emmanuel O. Olorunsola

    2017-01-01

    Full Text Available This study was aimed at evaluating chitosan-microcrystalline cellulose blends as direct compression excipients. Crab shell chitosan, α-lactose monohydrate, and microcrystalline cellulose powders were characterized. Blends of the microcrystalline cellulose and chitosan in ratios 9 : 1, 4 : 1, 2 : 1, and 1 : 1 as direct compression excipients were made to constitute 60% of metronidazole tablets. Similar tablets containing blends of the microcrystalline cellulose and α-lactose monohydrate as well as those containing pure microcrystalline cellulose were also produced. The compact density, tensile strength, porosity, disintegration time, and dissolution rate of tablets were determined. Chitosan had higher moisture content (7.66% and higher moisture sorption capacity (1.33% compared to microcrystalline cellulose and lactose. It also showed better flow properties (Carr’s index of 18.9% and Hausner’s ratio of 1.23. Compact density of tablets increased but tensile strength decreased with increase in the proportion of chitosan in the binary mixtures. In contrast to lactose, the disintegration time increased and the dissolution rate decreased with increase in the proportion of chitosan. This study has shown that chitosan promotes flowability of powder mix and rapid disintegration of tablet. However, incorporation of equal proportions of microcrystalline cellulose and chitosan leads to production of extended-release tablet. Therefore, chitosan promotes tablet disintegration at low concentration and enables extended-release at higher concentration.

  16. Dissolution process analysis using model-free Noyes-Whitney integral equation.

    Science.gov (United States)

    Hattori, Yusuke; Haruna, Yoshimasa; Otsuka, Makoto

    2013-02-01

    Drug dissolution process of solid dosages is theoretically described by Noyes-Whitney-Nernst equation. However, the analysis of the process is demonstrated assuming some models. Normally, the model-dependent methods are idealized and require some limitations. In this study, Noyes-Whitney integral equation was proposed and applied to represent the drug dissolution profiles of a solid formulation via the non-linear least squares (NLLS) method. The integral equation is a model-free formula involving the dissolution rate constant as a parameter. In the present study, several solid formulations were prepared via changing the blending time of magnesium stearate (MgSt) with theophylline monohydrate, α-lactose monohydrate, and crystalline cellulose. The formula could excellently represent the dissolution profile, and thereby the rate constant and specific surface area could be obtained by NLLS method. Since the long time blending coated the particle surface with MgSt, it was found that the water permeation was disturbed by its layer dissociating into disintegrant particles. In the end, the solid formulations were not disintegrated; however, the specific surface area gradually increased during the process of dissolution. The X-ray CT observation supported this result and demonstrated that the rough surface was dominant as compared to dissolution, and thus, specific surface area of the solid formulation gradually increased. Copyright © 2012 Elsevier B.V. All rights reserved.

  17. Impact of reducing and oxidising agents on the wheat flour dough dynamic rheological properties

    Directory of Open Access Journals (Sweden)

    Pavlína Pečivová

    2011-01-01

    Full Text Available Dynamic measurements with an oscillatory rheometer were made to study the rheological properties of wheat flour doughs and to examine how they are related to the composition of dough (the addition of oxidising and reducing agents.It was found that L-cysteine hydrochloride monohydrate (0.6 × 10−2 − 4.0 × 10−2 wt.%, L-cysteine p. a. (0.6 × 10−2 − 1.4 × 10−2 wt.% and glutathione-inactivated dry yeast (1.8 × 10−2 − 14.0 × 10−2 wt.% show softening effects. An interesting phenomenon was observed from the concentration of 2.4 × 10−2 wt.% of L-cysteine p. a., where proces of weakening was decelerated. L-cysteine start making cystine by reaction of two cysteine molecules and proces of weakening was decelerated. L-threonine, L-tryptophan within the concentration range of 2.0 × 10−2 − 14.0 × 10−2 wt.% and L-tyrosine, especially at concentrations 10.0 × 10−2 − 14.0 × 10−2 wt.%, have strengthening effects. L-cysteine hydrochloride monohydrate exhibited the strongest softening effect while L-tryptophan had the strongest stiffening effect on the gluten network.

  18. Potential of carrageenans to protect drugs from polymorphic transformation.

    Science.gov (United States)

    Schmidt, Andrea G; Wartewig, Siegfried; Picker, Katharina M

    2003-07-01

    Carrageenans were analysed in mixture with polymorphic drugs to test their potential for minimising polymorphic or pseudopolymorphic transitions, which are induced by the tableting process. The kappa-carrageenans Gelcarin GP-812 NF and Gelcarin GP-911 NF and the iota-carrageenan Gelcarin GP-379 NF were tested in comparison to the well-known tableting excipients microcrystalline cellulose (MCC), hydroxypropyl methylcellulose (HPMC), and dicalcium phosphate dihydrate (DCPD). Amorphous indomethacin was chosen as model drug since its well-known recrystallisation behaviour can be mechanically stimulated. Further on, theophylline monohydrate was used. Its dehydration is induced by tableting. Pure materials and mixtures containing 20% (w/w) drug were compressed up to different maximum relative densities. The data obtained during tableting were analysed by three-dimensional (3D) modelling. Afterwards tablets were broken and examined by Fourier transform Raman spectroscopy in order to determine the degree of transformation inside the tablet. For quantitative interpretation, the intensities of representative bands were used. Thermal analysis was used additionally. Using 3D modelling a decrease of plastic deformation can be noticed in the order HPMC>MCC>carrageenans, whereas DCPD represents an exception because of brittle fracture. Best hindrance of polymorphic transformation showed the carrageenans, the hindrance was slightly worse for HPMC. MCC and DCPD could not hinder transformation. A complete protection of the amorphous form could not be achieved. For theophylline monohydrate, the results were similar.

  19. Formation and Transformation Behavior of Sodium Dehydroacetate Hydrates

    Directory of Open Access Journals (Sweden)

    Xia Zhang

    2016-04-01

    Full Text Available The effect of various controlling factors on the polymorphic outcome of sodium dehydroacetate crystallization was investigated in this study. Cooling crystallization experiments of sodium dehydroacetate in water were conducted at different concentrations. The results revealed that the rate of supersaturation generation played a key role in the formation of the hydrates. At a high supersaturation generation rate, a new sodium dehydroacetate dihydrate needle form was obtained; on the contrary, a sodium dehydroacetate plate monohydrate was formed at a low supersaturation generation rate. Furthermore, the characterization and transformation behavior of these two hydrated forms were investigated with the combined use of microscopy, powder X-ray diffraction (PXRD, Raman spectroscopy, Fourier transform infrared (FTIR, thermal gravimetric analysis (TGA, scanning electron microscopy (SEM and dynamic vapor sorption (DVS. It was found that the new needle crystals were dihydrated and hollow, and they eventually transformed into sodium dehydroacetate monohydrate. In addition, the mechanism of formation of sodium dehydroacetate hydrates was discussed, and a process growth model of hollow crystals in cooling crystallization was proposed.

  20. Ceftriaxone-associated gallbladder sludge. Identification of calcium-ceftriaxone salt as a major component of gallbladder precipitate

    International Nuclear Information System (INIS)

    Park, H.Z.; Lee, S.P.; Schy, A.L.

    1991-01-01

    Ceftriaxone, a third-generation cephalosporin, is partially excreted into bile. With its clinical use, the formation of gallbladder sludge detected by ultrasonography has been reported. Four surgical specimens were examined and no gallstones were found. Instead, fine precipitates of 20-250 microns were present. Microscopically, there was a small number of cholesterol monohydrate crystals and bilirubin granules among an abundant amount of granular-crystalline material that was not morphologically cholesterol monohydrate crystals. The chemical composition of the precipitates (n = 4) was determined. There was a small amount of cholesterol (1.7% +/- 0.8%) and bilirubin (13.9% +/- 0.74%). The major component of the precipitate was a residue. On further analysis using thin-layer chromatography, high-performance liquid chromatography, and electron microprobe analysis, the residue was identified as a calcium salt of ceftriaxone. The residue also had identical crystal morphology and chromatographic elution profile as authentic calcium-ceftriaxone standards. It is concluded that ceftriaxone, after excretion and being concentrated in the gallbladder bile, can form a precipitate. The major constituent has been identified as a ceftriaxone-calcium salt

  1. Characterization of crystalline structures in Opuntia ficus-indica.

    Science.gov (United States)

    Contreras-Padilla, Margarita; Rivera-Muñoz, Eric M; Gutiérrez-Cortez, Elsa; del López, Alicia Real; Rodríguez-García, Mario Enrique

    2015-01-01

    This research studies the crystalline compounds present in nopal (Opuntia ficus-indica) cladodes. The identification of the crystalline structures was performed using X-ray diffraction, scanning electron microscopy, mass spectrometry, and Fourier transform infrared spectroscopy. The crystalline structures identified were calcium carbonate (calcite) [CaCO3], calcium-magnesium bicarbonate [CaMg(CO3)2], magnesium oxide [MgO], calcium oxalate monohydrate [Ca(C2O4)•(H2O)], potassium peroxydiphosphate [K4P2O8] and potassium chloride [KCl]. The SEM images indicate that calcite crystals grow to dipyramidal, octahedral-like, prismatic, and flower-like structures; meanwhile, calcium-magnesium bicarbonate structures show rhombohedral exfoliation and calcium oxalate monohydrate is present in a drusenoid morphology. These calcium carbonate compounds have a great importance for humans because their bioavailability. This is the first report about the identification and structural analysis of calcium carbonate and calcium-magnesium bicarbonate in nopal cladodes, as well as the presence of magnesium oxide, potassium peroxydiphosphate and potassium chloride in these plants. The significance of the study of the inorganic components of these cactus plants is related with the increasing interest in the potential use of Opuntia as a raw material of products for the food, pharmaceutical, and cosmetic industries.

  2. Fourier Transform Infrared Analysis of Urinary Calculi and Metabolic Studies in a Group of Sicilian Children.

    Science.gov (United States)

    D'Alessandro, Maria Michela; Gennaro, Giuseppe; Tralongo, Pietro; Maringhini, Silvio

    2017-05-01

    Prevalence of urinary calculi in children has been increasing in the past years. We performed an analysis of the chemical composition of stones formers of the pediatric population in our geographical area over the years 2005 to 2013. Fourier transform infrared spectroscopy was employed for the determination of the calculus composition of a group of Sicilian children, and metabolic studies were performed to formulate the correct diagnosis and establish therapy. The prevalence of stone formation was much higher for boys than for girls, with a sex ratio of 1.9:1. The single most frequent component was found to be calcium oxalate monohydrate, and calcium oxalates (pure or mixed calculi) were the overall most frequent components. Calcium phosphates ranked 2nd for frequency, most often in mixed calculi, while urates ranked 3rd. The metabolic disorder most often associated with pure calcium oxalate monohydrate calculi was hypocitraturia, while hyperoxaluria was predominantly associated with calcium oxalate dihydrate calculi. Mixed calculi had the highest prevalence in our pediatric population. Our data showed that Fourier transform infrared spectroscopy was a useful tool for the determination of the calculi composition.

  3. Gas adsorption on commercial magnesium stearate: Effects of degassing conditions on nitrogen BET surface area and isotherm characteristics.

    Science.gov (United States)

    Lapham, Darren P; Lapham, Julie L

    2017-09-15

    Commercial grades of magnesium stearate have been analysed by nitrogen adsorption having been pre-treated at temperatures between 30°C and 110°C and in the as-received state. Characteristics of nitrogen adsorption/desorption isotherms are assessed through the linearity of low relative pressure isotherm data and the BET transform plot together with the extent of isotherm hysteresis. Comparison is made between thermal gravimetric analysis and mass loss on drying. Features of gas adsorption isotherms considered atypical are identified and possible causes presented. It is shown that atypical isotherm features and issues of applying BET theory to the calculation of S BET are linked to the presence of hydrated water and that these depend on the hydration state: being more pronounced for the di-hydrate than the mono-hydrate. Dehydration reduces the extent of atypical features. S BET of a mono-hydrate sample is 5.6m 2 g -1 and 3.2m 2 g -1 at 40°C and 100°C degassing respectively but 23.9m 2 g 1 and 5.9m 2 g -1 for di-hydrate containing samples under comparable degassing. Di-hydrated samples also show S BET >15m 2 g 1 , BET C-values adsorption data. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Evaluation of low-dose dual energy computed tomography for in vivo assessment of renal/ureteric calculus composition.

    Science.gov (United States)

    Mahalingam, Harshavardhan; Lal, Anupam; Mandal, Arup K; Singh, Shrawan Kumar; Bhattacharyya, Shalmoli; Khandelwal, Niranjan

    2015-08-01

    This study aimed to assess the accuracy of low-dose dual-energy computed tomography (DECT) in predicting the composition of urinary calculi. A total of 52 patients with urinary calculi were scanned with a 128-slice dual-source DECT scanner by use of a low-dose protocol. Dual-energy (DE) ratio, weighted average Hounsfield unit (HU) of calculi, radiation dose, and image noise levels were recorded. Two radiologists independently rated study quality. Stone composition was assessed after extraction by Fourier transform infrared spectroscopy (FTIRS). Analysis of variance was used to determine if the differences in HU values and DE ratios between the various calculus groups were significant. Threshold cutoff values to classify the calculi into separate groups were identified by receiver operating characteristic curve analysis. A total of 137 calculi were detected. FTIRS analysis differentiated the calculi into five groups: uric acid (n=17), struvite (n=3), calcium oxalate monohydrate and dihydrate (COM-COD, n=84), calcium oxalate monohydrate (COM, n=28), and carbonate apatite (n=5). The HU value could differentiate only uric acid calculi from calcified calculi (p80% sensitivity and specificity to differentiate them. The DE ratio could not differentiate COM from COM-COD calculi. No study was rated poor in quality by either of the observers. The mean radiation dose was 1.8 mSv. Low-dose DECT accurately predicts urinary calculus composition in vivo while simultaneously reducing radiation exposure without compromising study quality.

  5. Weak interactions in clobazam–lactose mixtures examined by differential scanning calorimetry: Comparison with the captopril–lactose system

    International Nuclear Information System (INIS)

    Toscani, S.; Cornevin, L.; Burgot, G.

    2012-01-01

    Highlights: ► Thermodynamic and kinetic parameters of weak interactions in binary systems by DSC. ► Energy-barrier decrease for lactose dehydration induced by clobazam. ► Recrystallisation of metastable liquid clobazam induced by anhydrous alpha lactose. ► Decrease of lactose dehydration temperature in binary mixtures with captopril. ► Increase of lactose dehydration enthalpy in binary mixtures with captopril. - Abstract: The thermal behaviour of binary mixtures of two drugs (clobazam and captopril, respectively) and a pharmaceutical excipient (lactose monohydrate) was measured with differential scanning calorimetry to determine thermodynamic and kinetic parameters (dehydration and melting enthalpies and dehydration and glass-transition activation energies) which might be affected by intermolecular interactions. A kinetic study showed that lactose dehydration is not a single-step conversion and that clobazam contributed to reduce the energy barrier for the bulk dehydration of the excipient. On the other hand, the physical interactions between metastable liquid clobazam and crystalline anhydrous α-lactose obtained from monohydrate dehydration gave rise to the recrystallisation of clobazam. In the captopril–lactose system, the liquid captopril influenced the lactose dehydration: a sharp increase of the dehydration enthalpy and a concurrent reduction of the dehydration temperature were observed. Finally, it turned out that solid-phase transitions were enhanced by the contact with a liquid phase.

  6. Characterization of the lanthanum(III) and europium(III) trichloroacetate complexes extracted with 18-crown-6

    International Nuclear Information System (INIS)

    Imura, H.; Saito, Y.; Ohashi, K.; Meguro, Y.; Yoshida, Z.; Choppin, G.R.

    1996-01-01

    Extraction of lanthanide(III) ions with 18-crown-6 (18C6) and trichloroacetate (tca) has been studied. The composition, hydration, and structure of the La(III) and Eu(III) complexes extracted into 1,2-dichloroethane were investigated by using several methods such as the liquid-liquid distribution technique, conductimetry, Karl Fisher titration, laser luminescence spectroscopy, and 1 H NMR. The La(III) complex was found to be a monohydrate, La(tca) 3 (18C6)(H 2 O), while that of Eu(III) was a mixture of a monohydrate and a dihydrate, i.e., Eu(tca) 3 (18C6)(H 2 O) and Eu(tca) 3 (18C6)(H 2 O) 2 . The origin of the selectivity by 18C6 which gives much higher extractability of La(III) than of Eu(III) is explained by considering the hydration and probable structure of their complexes. 12 refs., 5 figs., 4 tabs

  7. FT-Raman and FT-IR studies of 1:2.5 piroxicam: β-cyclodextrin inclusion compound

    Science.gov (United States)

    Bertoluzza, A.; Rossi, M.; Taddei, P.; Redenti, E.; Zanol, M.; Ventura, P.

    1999-05-01

    The FT-Raman and FT-IR spectra of amorphous 1:2.5 piroxicam (P): β-cyclodextrin (βCD) inclusion compound (PβCD) are presented and discussed in comparison with the spectra of the three main modifications of piroxicam (α,β and monohydrate). In the 1700-1200 cm -1 FT-Raman spectrum of 1:2.5 PβCD inclusion compound the bands of βCD are weak and covered by those stronger of piroxicam, differently from the FT-IR spectrum where the bands of βCD are stronger, so covering a large part of the spectrum. Typical FT-Raman marker bands are assigned for the characterization of the three modifications of piroxicam. The FT-Raman spectrum of 1:2.5 PβCD inclusion compound predominantly shows the bands at about 1465 and 1400 cm -1 of the monohydrate, indicating that piroxicam assumes the zwitterionic structure stabilized by interaction with βCD via electrostatic and hydrogen bonds. The dipolar character of 1:2.5 PβCD inclusion compound improves the solubility and the dissolution rate of piroxicam and thus its rate of absorption.

  8. Bone regeneration in cranioplasty and clinical complications in rabbits with alloxan-induced diabetes

    Directory of Open Access Journals (Sweden)

    Evanice Menezes Marçal Vieira

    2008-06-01

    Full Text Available This research evaluated the bone repair process in surgical defects created on the parietal bones of diabetic rabbits using the guided bone regeneration technique to observe the effects of alloxan in the induction of diabetes mellitus. Twenty-four adult rabbits were divided into three study groups: control (C, diabetic (D and diabetic associated to polytetrafluoroethylene (PTFE membrane (D-PTFE. For diabetes induction the animals received one dose of monohydrated alloxan (90 mg/kg by intravenous administration in the auricular or femoral vein. In group D-PTFE the membrane covered both the floor and the surface of the bone defect. In groups D and C, the bone defect was filled up with blood clot. The specimens were fixed in 10% formol and prepared for histomorphometric analysis. The results showed that the 90 mg/kg dose of monohydrate alloxan was sufficient to promote diabetes mellitus when administered in the auricular vein. Bone regeneration was slower in the diabetic group when compared with the control and diabetic-PTFE groups, but there was no significant statistical difference between the two experimental groups (D and D-PTFE. The oral and general clinical complications among the diabetics were weight loss, polyuria, polyphagia and severe chronic gingivitis.

  9. Protonation of inorganic 5-Fluorocytosine salts

    Science.gov (United States)

    Souza, Matheus S.; da Silva, Cecília C. P.; Almeida, Leonardo R.; Diniz, Luan F.; Andrade, Marcelo B.; Ellena, Javier

    2018-06-01

    5-Fluorocytosine (5-FC) has been widely used for the treatment of fungal infections and recently was found to exert an extraordinary antineoplastic activity in gene directed prodrug therapy. However, despite of its intense use, 5-FC exhibits tabletability issues due its physical instability in humid environments, leading to transition from the anhydrous to monohydrate phase. By considering that salt formation is an interesting strategy to overcome this problem, in this paper crystal engineering approach was applied to the supramolecular synthesis of new 5-FC salts with sulfuric, hydrobromic and methanesulfonic inorganic acids. A total of four structures were obtained, namely 5-FC sulfate monohydrate (1:1:1), 5-FC hydrogen sulfate (1:1), 5-FC mesylate (1:1) and 5-FC hydrobromide (1:1), the last one being a polymorphic form of a structure already reported in the literature. These novel salts were structurally characterized by single crystal X-ray diffraction and its supramolecular organization were analyses by Hirshfeld surface analysis. The vibrational behavior was evaluated by Raman spectroscopy and it was found to be consistent with the crystal structures.

  10. The standard enthalpies of formation of L-asparagine and L-{alpha}-glutamine

    Energy Technology Data Exchange (ETDEWEB)

    Contineanu, Iulia, E-mail: icontineanu@yahoo.com [Institute of Physical Chemistry ' I.G. Murgulescu' , Spl. Independentei 202, Bucharest (Romania); Neacsu, Ana, E-mail: anna_matache@yahoo.com [Institute of Physical Chemistry ' I.G. Murgulescu' , Spl. Independentei 202, Bucharest (Romania); Perisanu, Stefan T., E-mail: stefan.perisanu@upb.ro [Laboratory of General Chemistry, Polytechnic University of Bucharest, str. Polizu nr. 1, Bucuresti (Romania)

    2010-01-10

    The energies of combustion of L-asparagine and L-{alpha}-glutamine were measured in a static bomb adiabatic calorimeter. Corrections were made for the heats due to the ignition of sample and for the nitric acid formation. The derived enthalpies of formation in solid state of asparagine monohydrate, nonhydrated asparagine and glutamine are respectively -1084.1 {+-} 3.0, -788.1 {+-} 4.7 and -834.3 {+-} 4.6 kJ mol{sup -1}. The data of enthalpy of formation are compared with the literature values and with estimated values by means of group additivity, using parameters recommended by Domalski and Hearing. The discrepancies between experimental and calculated values are explained by considering the number and strength of intermolecular hydrogen bonds. The dehydration of asparagine monohydrate and the possible melting of the three amino acids were investigated by means of DSC. Glutamine melts without considerable decomposition at about 182 {sup o}C, while asparagines decompose during the fusion process (208 {sup o}C).

  11. The experimental charge-density approach in the evaluation of intermolecular interactions. Application of a new module of the XD programming package to several solids including a pentapeptide.

    Science.gov (United States)

    Abramov, Y A; Volkov, A; Wu, G; Coppens, P

    2000-11-01

    A new module interfaced to the XD programming package has been used in the evaluation of intermolecular interactions and lattice energies of the crystals of p-nitroaniline, L-asparagine monohydrate and the pentapeptide Boc-Gln-D-Iva-Hyp-Ala-Phol (Boc = butoxycarbonyl, Iva = isovaline = ethylalanine, Phol = phenylalaninol). The electrostatic interactions are evaluated with the atom-centered distributed multipoles from KRMM (kappa'-restricted multipole model) refinements, using the Buckingham expression for non-overlapping charge densities. Results for p-nitroaniline are compared with Hartree-Fock (HF), density functional (DFT) and Moller-Plesset (MP2) supermolecular calculations and with HF and DFT periodic calculations. The HF and DFT methods fail to predict the stability of the p-nitroaniline crystal but the results of the experimental charge-density approach (ECDA) are in good agreement with both MP2 interaction energies and the experimental lattice energy. ECDA results for L-asparagine monohydrate compare well with those from DFT supermolecular and periodic HF calculations. The disorder of the terminal group in the pentapeptide, which persists at the experimental temperature of 20 K, corresponds to an energy difference of only 0.35 kJ mol(-1), which is too small to be reproduced with current methods.

  12. Gateways to clinical trials.

    Science.gov (United States)

    Tomillero, A; Moral, M A

    2009-05-01

    (-)-Gossypol; Abacavir sulfate/lamivudine, ACAM-1000, ACE-011, Agomelatine, AGS-004, Alemtuzumab, Alvocidib hydrochloride, AMG-317, Amlodipine, Aripiprazole, Atazanavir sulfate, Azacitidine; Becatecarin, Belinostat, Bevacizumab, BMS-387032, BMS-690514, Bortezomib; Casopitant mesylate, Cetuximab, Choline fenofibrate, CK-1827452, Clofarabine, Conivaptan hydrochloride; Dabigatran etexilate, DADMe-Immucillin-H, Darbepoetin alfa, Darunavir, Dasatinib, DC-WT1, Decitabine, Deferasirox, Degarelix acetate, Denenicokin, Denosumab, Dienogest, Duloxetine hydrochloride; Ecogramostim, Eculizumab, Edoxaban tosilate, Elacytarabine, Elesclomol, Eltrombopag olamine, Enfuvirtide, Enzastaurin hydrochloride, Eribulin mesilate, Erlotinib hydrochloride, Escitalopram oxalate, Eszopiclone, Etravirine; Flibanserin, Fludarabine, Fondaparinux sodium, Fosamprenavir calcium; Gefitinib, Genistein; I-131-L19-SIP, Idrabiotaparinux sodium, Imatinib mesylate, IMGN-901, Ipilimumab; Laromustine, Lenalidomide, Liposomal cisplatin, Liraglutide, Lisdexamfetamine mesilate, Lopinavir, Lopinavir/ritonavir; Maraviroc, MDV-3100, Mecasermin rinfabate, MP-470, Mycophenolic acid sodium salt; Naproxcinod, NB-002, Nesiritide, Nilotinib hydrochloride monohydrate, NK-012; Palonosetron hydrochloride, Panobinostat, Pegfilgrastim, Peginterferon alfa-2a, Pitavastatin calcium, PL-3994, Plerixafor hydrochloride, Plitidepsin, PM-10450; Raltegravir potassium, Recombinant human soluble thrombomodulin, ReoT3D, RHAMM R3 peptide, Rivaroxaban, Romiplostim, Rosuvastatin calcium, Rozrolimupab; Sabarubicin hydrochloride, Salinosporamide A, Sirolimus-eluting stent, Smallpox (Vaccinia) Vaccine, Live, Sorafenib; Tenofovir disoproxil fumarate, Tenofovir disoproxil fumarate/emtricitabine, Teriparatide, Tipifarnib, Tipranavir, Trabectedin, Trifluridine/TPI; Vardenafil hydrochloride hydrate, Vinflunine, Volociximab, Vorinostat; Ximelagatran; Yttrium 90 (90Y) ibritumomab tiuxetan; Ziprasidone hydrochloride, Zoledronic acid monohydrate

  13. Temperature dependence of the heat capacities in the solid state of 18 mono-, di-, and poly-saccharides

    International Nuclear Information System (INIS)

    Hernandez-Segura, Gerardo O.; Campos, Myriam; Costas, Miguel; Torres, Luis A.

    2009-01-01

    The temperature dependence of the heat capacities in solid state C p (T) of 18 mono-, di-, and poly-saccharides has been determined using a power-compensation differential scanning calorimeter. The saccharides were α-D-xylose, D-ribose, 2-deoxy-D-ribose, methyl-β-D-ribose, α-D-glucose, 2-deoxy-D-glucose, α-D-mannose, β-D-fructose, α-D-galactose, methyl-α-D-glucose, sucrose, maltose monohydrate, α-lactose monohydrate, cellobiose, maltotriose, N-acetyl-D-glucosamine, α-cyclodextrin, and β-cyclodextrin. The measurements were carried out at atmospheric pressure and from T = (288.15 to 358.15) K for 15 saccharides and from T = (288.15 to 328.15) K for D-ribose, 2-deoxy-D-ribose, and methyl-β-D-ribose. The present results are compared against literature values both at single temperatures, where most of the data are available, and throughout a range of temperatures, i.e., for C p (T). The predictions of a recently published correlation for organic solids are briefly discussed. By grouping saccharides in subsets, our present results can be used to compare amongst saccharide isomers and to assess the effect of different chemical groups and molecular size

  14. Quantitative Mineralogical Composition of Calculi and Urine Abnormalities for Calcium Oxalate Stone Formers: A Single-Center Results.

    Science.gov (United States)

    Kustov, Andrey V; Strelnikov, Alexander I

    2017-12-26

    The paper focuses on the relationship of risk factors and metabolic disorders with mineralogical composition of calculi, age and gender of calcium oxalate stone formers. Stone mineralogical composition, 24 hour biochemistry and pH-profile of urine were examined for sixty four stone formers using powder X-ray diffraction, spectrophotometric and potentiometric techniques. The analysis indicated that 44 % of calculi were composed of pure calcium oxalate monohydrate, whereas other 56 % contained both monohydrate and dihydrate or usually their mixtures with hydroxyl apatite. Hypocitraturia, hypercalciuria and hyperuricosuria were identified as the most frequent disorders. Patients with pure calcium oxalate stones and calcium oxalate mixed with apatite revealed different patterns including age, acid-base balance of urine, calcium, citrate excretion etc. Our results demonstrate that most patients simultaneously reveal several risk factors. The special attention should be paid to normalize the daily citrate, calcium and urate excretion. High risk patients, such as postmenopausal females or stone formers with a high apatite content require a specific metabolic evaluation towards in highlighting abnormalities associated with stone formation.

  15. Organogel-emulsions with mixtures of β-sitosterol and γ-oryzanol: influence of water activity and type of oil phase on gelling capability.

    Science.gov (United States)

    Sawalha, Hassan; den Adel, Ruud; Venema, Paul; Bot, Arjen; Flöter, Eckhard; van der Linden, Erik

    2012-04-04

    In this study, water-in-oil emulsions were prepared from water containing different salt concentrations dispersed in an oil phase containing a mixture of β-sitosterol and γ-oryzanol. In pure oil, the β-sitosterol and γ-oryzanol molecules self-assemble into tubular microstructures to produce a firm organogel. However, in the emulsion, the water molecules bind to the β-sitosterol molecules, forming monohydrate crystals that hinder the formation of the tubules and resulting in a weaker emulsion-gel. Addition of salt to the water phase decreases the water activity, thereby suppressing the formation of sitosterol monohydrate crystals even after prolonged storage times (∼1 year). When the emulsions were prepared with less polar oils, the tubular microstructure was promoted, which significantly increased the firmness of the emulsion-gel. The main conclusion of this study is that the formation of oryzanol and sitosterol tubular microstructure in the emulsion can be promoted by reducing the water activity and/or by using oils of low polarity.

  16. Preparation and in vitro/in vivo evaluation of antimicrobial ocular in situ gels containing a disappearing preservative for topical treatment of bacterial conjunctivitis.

    Science.gov (United States)

    Saher, Osama; Ghorab, Dalia M; Mursi, Nadia M

    2016-08-01

    The study aimed to formulate and evaluate levofloxacin hemihydrate ocular in situ gels along with freshly prepared disappearing preservative reported to be safer to human eyes. Formulae were prepared using thermosensitive (PF127 and PF68) or ion-activated (Gelrite) polymers. They were evaluated for gelation temperature (GT), capacity, content uniformity, pH, rheological behavior, in vitro drug release with kinetic analysis. Best formulae were exposed to storage effect to select the optimum formula that was subjected to different sterilization methods and in vivo evaluation. The prepared disappearing preservative (sodium perborate monohydrate) proved to be active oxidative preservative and compatible with our formulae. F9 (24% PF127, 15% PF 68, 0.5% levofloxacin hemihydrate, and 0.0025% sodium perborate monohydrate) showed prolonged drug release (12 h), acceptable GT, viscosity, and pH. It remained stable over 3 months at two temperatures and was best sterilized by filtration. It showed longer residence time (12 h) in rabbits' eye fluids compared with the Levoxin® eye drops (4 h). This successful attempt of using thermo-gelling system along with a disappearing type of preservatives would allow the use of these systems to achieve sustained release of antimicrobial drugs with minimum risk of eye damage improving patient compliance and treatment efficacy.

  17. Creatine and creatine forms intended for sports nutrition.

    Science.gov (United States)

    Andres, Susanne; Ziegenhagen, Rainer; Trefflich, Iris; Pevny, Sophie; Schultrich, Katharina; Braun, Hans; Schänzer, Wilhelm; Hirsch-Ernst, Karen Ildico; Schäfer, Bernd; Lampen, Alfonso

    2017-06-01

    Creatine is a popular ergogenic supplement in sports nutrition. Yet, supplementation of creatine occasionally caused adverse effects such as gastrointestinal complaints, muscle cramps and an increase in body weight. Creatine monohydrate has already been evaluated by different competent authorities and several have come to the conclusion that a daily intake of 3 g creatine per person is unlikely to pose safety concerns, focusing on healthy adults with exclusion of pregnant and breastfeeding women. Possible vulnerable subgroups were also discussed in relation to the safety of creatine. The present review provides an up-to-date overview of the relevant information with special focus on human studies regarding the safety of creatine monohydrate and other marketed creatine forms, in particular creatine pyruvate, creatine citrate, creatine malate, creatine taurinate, creatine phosphate, creatine orotate, creatine ethyl ester, creatine pyroglutamate, creatine gluconate, and magnesium creatine chelate. Limited data are available with regard to the safety of the latter creatine forms. Considering an acceptable creatine intake of 3 g per day, most of the evaluated creatine forms are unlikely to pose safety concerns, however some safety concerns regarding a supplementary intake of creatine orotate, creatine phosphate, and magnesium creatine chelate are discussed here. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Preventing Crystal Agglomeration of Pharmaceutical Crystals Using Temperature Cycling and a Novel Membrane Crystallization Procedure for Seed Crystal Generation

    Directory of Open Access Journals (Sweden)

    Elena Simone

    2018-01-01

    Full Text Available In this work, a novel membrane crystallization system was used to crystallize micro-sized seeds of piroxicam monohydrate by reverse antisolvent addition. Membrane crystallization seeds were compared with seeds produced by conventional antisolvent addition and polymorphic transformation of a fine powdered sample of piroxicam form I in water. The membrane crystallization process allowed for a consistent production of pure monohydrate crystals with narrow size distribution and without significant agglomeration. The seeds were grown in 350 g of 20:80 w/w acetone-water mixture. Different seeding loads were tested and temperature cycling was applied in order to avoid agglomeration of the growing crystals during the process. Focused beam reflectance measurement (FBRM; and particle vision and measurement (PVM were used to monitor crystal growth; nucleation and agglomeration during the seeded experiments. Furthermore; Raman spectroscopy was used to monitor solute concentration and estimate the overall yield of the process. Membrane crystallization was proved to be the most convenient and consistent method to produce seeds of highly agglomerating compounds; which can be grown via cooling crystallization and temperature cycling.

  19. Performance indicators for carrier-based DPIs: Carrier surface properties for capsule filling and API properties for in vitro aerosolisation.

    Science.gov (United States)

    Faulhammer, E; Zellnitz, S; Wutscher, T; Stranzinger, S; Zimmer, A; Paudel, A

    2018-01-30

    This study investigates engineered carrier, as well as engineered API particles, and shows that there are distinct performance indicators of particle engineering for carrier-based dry powder inhalers (DPIs). Spray dried (SDSS) and jet-milled (JMSS) salbutamol sulphate (SS) was blended with untreated α-lactose monohydrate (LAC_R) and α-lactose monohydrate engineered (LAC_E). Subsequent capsule filling was performed with different process settings on a dosator nozzle capsule filling machine in order to reach a target fill weight of 20-25 mg. To evaluate the performance of the different mixtures, in vitro lung deposition experiments were carried out with a next generation impactor, the emitted dose (ED) and fine particle fraction (FPF) were calculated based on the specification of the European pharmacopoeia. The FPF of micronised powder blends is significantly higher (20%) compared to the FPF of spray dried blends (5%). Compared to API engineering, carrier engineering had a positive effect on the capsule filling performance (weight variability and mean fill weight) at lower compression ratios (setting 1). Results further showed that higher compression ratios appear to be beneficial in terms of capsule filling performance (higher fill weight and less fill weight variation). Concluding, it can be stated that the carrier engineering, or generally carrier properties, govern downstream processing, whereas the API engineering and API properties govern the aerosolisation performance and thereby significantly affect the dose delivery to the lungs. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. Weak interactions in clobazam-lactose mixtures examined by differential scanning calorimetry: Comparison with the captopril-lactose system

    Energy Technology Data Exchange (ETDEWEB)

    Toscani, S. [Departement de Chimie - UMR 6226, Faculte des Sciences, Universite de Rennes 1, Batiment 10B, 263 avenue du General Leclerc, F-35042 Rennes Cedex (France); Cornevin, L. [Universite de Rennes 1, Faculte de Pharmacie, 2 Avenue Leon Bernard, F-35043 Rennes Cedex (France); Burgot, G., E-mail: Gwenola.burgot@univ-rennes1.fr [Universite de Rennes 1, Faculte de Pharmacie, Laboratoire de Chimie Analytique, EA 1274 ' Mouvement, sports, sante' , 2 Avenue Leon Bernard, F-35043 Rennes Cedex (France); CHGR Rennes, Pole Medico-Technique Pharmacie, F-35703 Rennes Cedex (France)

    2012-09-10

    Highlights: Black-Right-Pointing-Pointer Thermodynamic and kinetic parameters of weak interactions in binary systems by DSC. Black-Right-Pointing-Pointer Energy-barrier decrease for lactose dehydration induced by clobazam. Black-Right-Pointing-Pointer Recrystallisation of metastable liquid clobazam induced by anhydrous alpha lactose. Black-Right-Pointing-Pointer Decrease of lactose dehydration temperature in binary mixtures with captopril. Black-Right-Pointing-Pointer Increase of lactose dehydration enthalpy in binary mixtures with captopril. - Abstract: The thermal behaviour of binary mixtures of two drugs (clobazam and captopril, respectively) and a pharmaceutical excipient (lactose monohydrate) was measured with differential scanning calorimetry to determine thermodynamic and kinetic parameters (dehydration and melting enthalpies and dehydration and glass-transition activation energies) which might be affected by intermolecular interactions. A kinetic study showed that lactose dehydration is not a single-step conversion and that clobazam contributed to reduce the energy barrier for the bulk dehydration of the excipient. On the other hand, the physical interactions between metastable liquid clobazam and crystalline anhydrous {alpha}-lactose obtained from monohydrate dehydration gave rise to the recrystallisation of clobazam. In the captopril-lactose system, the liquid captopril influenced the lactose dehydration: a sharp increase of the dehydration enthalpy and a concurrent reduction of the dehydration temperature were observed. Finally, it turned out that solid-phase transitions were enhanced by the contact with a liquid phase.

  1. Prediction of successful treatment by extracorporeal shock wave lithotripsy based on crystalluriacomposition correlations of urinary calculi

    Directory of Open Access Journals (Sweden)

    Nadia Messaoudi

    2015-12-01

    Full Text Available Objective: To provide correlations between crystalluria and chemical structure of calculi in situ to help making decision in the use of the extracorporeal shock wave lithotripsy (ESWL. Methods: A crystalluria study was carried out on 644 morning urines of 172 nephrolithiasis patients (111 males and 61 females, and 235 of them were in situ stone carriers. After treating by ESWL, the recovered calculi have been analyzed by Fourier transform infrared spectroscopy and their compositions were correlated to the nature of urinary crystals. Results: We obtained successful treatment for 109 patients out of 157 and 63 patients out of 78 with stones had a treatment failure (33.2%. The correlations showed that for the overwhelming crystalluria containing calcium oxalate dihydrate (COD with mixed crystals without calcium oxalate monohydrate, we should have 68% to 88 % success rate. However, the obtained result was 79%. Similarly, for crystalluria with COD + calcium oxalate monohydrate ± carbapatite, the prediction was 11% to 45% and the result was approximately 39%. When the majority of crystalluria was calcium phosphate, the prediction of 50% to 80% was confirmed by 71% success rate. For those majority containing magnesium ammonium phosphate hexahydrate (struvite ± diammonium urate ± COD, we predicted between 80% to 100%, and the result gave a success rate of 84%. Conclusions: The analysis of crystalluria of morning urine can help to know the composition of calculi in situ and can predict the success rate of ESWL for maximum efficiency.

  2. Rotational Spectrum of the Methyl Salicylate-Water Complex: the Missing Conformer and the Tunneling Motions

    Science.gov (United States)

    Ghosh, Supriya; Thomas, Javix; Xu, Yunjie; Jäger, Wolfgang

    2015-06-01

    Methyl salicylate is a naturally occurring organic ester produced by wintergreen and other plants. It is also found in many over-the-counter remedies, such as muscle ache creams. The rotational spectrum of the methyl salicylate monomer was reported previously, where the most stable, dominant conformer was identified. The methyl salicylate-water complex was first studied using fluorescence-detected infrared spectroscopy; only one monohydrate conformer was found in that work. In the present study, we employed both broadband chirped and cavity based Fourier transform microwave spectroscopy to examine the competition between intra- and intermolecular hydrogen-bonding interactions and possible large amplitude motions associated with the methyl group and the water subunit. In contrast to the previous infrared study, two monohydrate conformers were identified, with carbonyl O or hydroxyl O as the hydrogen bond acceptors. Detailed analyses of the observed hyperfine structures will be presented, as well as our efforts to extend the study to larger methyl salicylate hydration clusters. S. Melandri, B. M. Giuliano, A. Maris, L. B. Favero, P. Ottaviani, B. Velino, W. Caminati, J. Phys. Chem. A. 2007, 111, 9076. A. Mitsuzuka, A. Fujii, T. Ebata, N. Mikami, J. Phys. Chem. A 1998, 102, 9779.

  3. Effects of creatine supplementation on oxidative stress profile of athletes

    Science.gov (United States)

    2012-01-01

    Background Creatine (Cr) supplementation has been widely used among athletes and physically active individuals. Secondary to its performance-enhancing ability, an increase in oxidative stress may occur, thus prompting concern about its use. The purpose of this study is to investigate the effects of Cr monohydrate supplementation and resistance training on muscle strength and oxidative stress profile in healthy athletes. Methods A randomized, double-blind, placebo-controlled method was used to assess twenty-six male elite Brazilian handball players divided into 3 groups: Cr monohydrate supplemented group (GC, N = 9), placebo group (GP, N = 9), no treatment group (COT, N = 8) for 32 days. All subjects underwent a resistance training program. Blood samples were drawn on 0 and 32 days post Cr supplementation to analyze the oxidative stress markers, thiobarbituric acid reactive species (TBARS), total antioxidant status (TAS), and uric acid. Creatine phosphokinase, urea, and creatinine were also analyzed, as well. Fitness tests (1 repetition maximum - 1RM and muscle endurance) were performed on the bench press. Body weight and height, body fat percentage (by measuring skin folds) and upper muscular area were also evaluated. Statistical analysis was performed using ANOVA. Results Only GC group showed increase in 1RM (54 ± 9 vs. 63 ± 10 kg; p = 0.0356) and uric acid (4.6 ± 1.0 vs. 7.4 ± 1.6 mg/dl; p = 0.025), with a decrease in TAS (1.11 ± 0.34 vs. 0.60 ± 0.19 mmol/l; p = 0.001). No differences (pre- vs. post-training) in TBARS, creatine phosphokinase, urea, creatinine, body weight and height, body fat percentage, or upper muscular area were observed in any group. When compared to COT, GC group showed greater decrease in TAS (−0.51 ± 0.36 vs. -0.02 ± 0.50 mmol/l; p = 0.0268), higher increase in 1RM (8.30 ± 2.26 vs. 5.29 ± 2.36 kg; p = 0.0209) and uric acid (2.77 ± 1.70 vs. 1.00 ± 1.03 mg/dl; p = 0.0276). Conclusion We conclude that Cr monohydrate

  4. Interaction of cephalosporin drugs with dodecyltrimethylammonium Bromide

    International Nuclear Information System (INIS)

    Hoque, Md. Anamul; Hossain, Mohammed Delwar; Khan, Mohammed Abdullah

    2013-01-01

    Highlights: • We carry out the interaction of cephalosporin drugs with DTAB conductometrically. • We examine the effect of drugs on the critical micelle concentration of DTAB. • Three critical micelle concentrations are obtained for drug- DTAB system. • Electrostatic and hydrophobic interactions between drugs and DTAB are proposed. • Drug supported micelle formation of DTAB is much favoured in aq. solution of K 2 SO 4 . -- Abstract: The interaction of three cephalosporin drugs namely cefadroxyl monohydrate (CFM), cephalexin monohydrate (CLM) and cephradine monohydrate (CDM) with dodecyltrimethylammonium Bromide (DTAB) has been carried out by conductance measurements in aqueous medium and in aqueous solution of K 2 SO 4 salt over temperature range of (303.15 to 318.15) K. For pure DTAB and drug-DTAB systems, three critical micelle concentrations were obtained. The third critical micelle concentration (c ∗ 3 ) indicates that the spherical micelle turns into rod shape that is sphere to rod transition. The c ∗ values of DTAB are changed due to the addition of cephalosporin drugs. In addition, the change of the values of c ∗ 1 , c ∗ 2 and c ∗ 3 with increase of the concentration of drugs indicate the presence of interaction between drug and DTAB. The c ∗ values indicate that micellization for the cephalosporins-surfactant systems in water follow the order: CFM-surfactant ∗ values for the cephalosporins - DTAB systems in aqueous K 2 SO 4 are lower in magnitude than those in pure water and the values decrease with increase of the concentrations of K 2 SO 4 at a particular temperature. A significant decrease of c ∗ values in the presence of K 2 SO 4 for cephalosporins-DTAB systems indicates that drug supported ionic micelle formation is much favoured in aqueous K 2 SO 4 solution compared to that in pure water. For cephalosporin-DTAB systems, ΔG 0 m values are negative which indicate that the drugs mediated ionic micelle formation processes are

  5. A Pilot Study of Creatine as a Novel Treatment for Depression in Methamphetamine Using Females

    Science.gov (United States)

    Hellem, Tracy L.; Sung, Young-Hoon; Shi, Xian-Feng; Pett, Marjorie A.; Latendresse, Gwen; Morgan, Jubel; Huber, Rebekah S.; Kuykendall, Danielle; Lundberg, Kelly J.; Renshaw, Perry F.

    2015-01-01

    Objective Depression among methamphetamine users is more prevalent in females than males, but gender specific treatment options for this comorbidity have not been described. Reduced brain phosphocreatine levels have been shown to be lower in female methamphetamine users compared to males, and, of relevance, studies have demonstrated an association between treatment resistant depression and reduced brain phosphocreatine concentrations. The nutritional supplement creatine monohydrate has been reported to reduce symptoms of depression in female adolescents and adults taking antidepressants, as well as to increase brain phosphocreatine in healthy volunteers. Therefore, the purpose of this pilot study was to investigate creatine monohydrate as a treatment for depression in female methamphetamine users. Methods Fourteen females with depression and comorbid methamphetamine dependence were enrolled in an 8 week open label trial of 5 grams of daily creatine monohydrate and of these 14, eleven females completed the study. Depression was measured using the Hamilton Depression Rating Scale (HAMD) and brain phosphocreatine levels were measured using phosphorus magnetic resonance spectroscopy pre- and post-creatine treatment. Secondary outcome measures included anxiety symptoms, measured with the Beck Anxiety Inventory (BAI), as well as methamphetamine use, monitored by twice weekly urine drug screens and self-reported use. Results The results of a linear mixed effects repeated measures model showed significantly reduced HAMD and BAI scores as early as week 2 when compared to baseline scores. This improvement was maintained through study completion. Brain phosphocreatine concentrations were higher at the second phosphorus magnetic resonance spectroscopy scan compared to the baseline scan; Mbaseline = 0.223 (SD = 0.013) vs. Mpost-treatment = 0.233 (SD = 0.009), t(9) = 2.905, p creatine increased phosphocreatine levels. Also, a reduction in methamphetamine positive urine drug

  6. Effects of creatine supplementation on oxidative stress profile of athletes

    Directory of Open Access Journals (Sweden)

    Percário Sandro

    2012-12-01

    Full Text Available Abstract Background Creatine (Cr supplementation has been widely used among athletes and physically active individuals. Secondary to its performance-enhancing ability, an increase in oxidative stress may occur, thus prompting concern about its use. The purpose of this study is to investigate the effects of Cr monohydrate supplementation and resistance training on muscle strength and oxidative stress profile in healthy athletes. Methods A randomized, double-blind, placebo-controlled method was used to assess twenty-six male elite Brazilian handball players divided into 3 groups: Cr monohydrate supplemented group (GC, N = 9, placebo group (GP, N = 9, no treatment group (COT, N = 8 for 32 days. All subjects underwent a resistance training program. Blood samples were drawn on 0 and 32 days post Cr supplementation to analyze the oxidative stress markers, thiobarbituric acid reactive species (TBARS, total antioxidant status (TAS, and uric acid. Creatine phosphokinase, urea, and creatinine were also analyzed, as well. Fitness tests (1 repetition maximum - 1RM and muscle endurance were performed on the bench press. Body weight and height, body fat percentage (by measuring skin folds and upper muscular area were also evaluated. Statistical analysis was performed using ANOVA. Results Only GC group showed increase in 1RM (54 ± 9 vs. 63 ± 10 kg; p = 0.0356 and uric acid (4.6 ± 1.0 vs. 7.4 ± 1.6 mg/dl; p = 0.025, with a decrease in TAS (1.11 ± 0.34 vs. 0.60 ± 0.19 mmol/l; p = 0.001. No differences (pre- vs. post-training in TBARS, creatine phosphokinase, urea, creatinine, body weight and height, body fat percentage, or upper muscular area were observed in any group. When compared to COT, GC group showed greater decrease in TAS (−0.51 ± 0.36 vs. -0.02 ± 0.50 mmol/l; p = 0.0268, higher increase in 1RM (8.30 ± 2.26 vs. 5.29 ± 2.36 kg; p = 0.0209 and uric acid (2.77 ± 1.70 vs. 1.00 ± 1.03 mg/dl; p = 0.0276. Conclusion We conclude that Cr

  7. Nanoscale observations of the effect of citrate on calcium oxalate precipitation on calcite surfaces.

    Science.gov (United States)

    Burgos-Cara, Alejandro; Ruiz-Agudo, Encarnacion; Putnis, Christine V.

    2016-04-01

    Calcium oxalate (CaC2O4ṡxH2O) minerals are naturally occurring minerals found in fossils, plants, kidney stones and is a by-product in some processes such as paper, food and beverage production [1,2]. In particular, calcium oxalate monohydrate phase (COM) also known as whewellite (CaC2O4ṡH2O), is the most frequently reported mineral phase found in urinary and kidney stones together with phosphates. Organic additives are well known to play a key role in the formation of minerals in both biotic and abiotic systems, either facilitating their precipitation or hindering it. In this regard, recent studies have provided direct evidence demonstrating that citrate species could enhance dissolution of COM and inhibit their precipitation. [3,4] The present work aims at evauate the influence of pH, citrate and oxalic acid concentrations in calcium oxalate precipitation on calcite surfaces (Island Spar, Chihuahua, Mexico) through in-situ nanoscale observation using in situ atomic force microscopy (AFM, Multimode, Bruker) in flow-through experiments. Changes in calcium oxalate morphologies and precipitated phases were observed, as well as the inhibitory effect of citrate on calcium oxalate precipitation, which also lead to stabilization an the amorphous calcium oxalate phase. [1] K.D. Demadis, M. Öner, Inhibitory effects of "green"additives on the crystal growth of sparingly soluble salts, in: J.T. Pearlman (Ed.), Green Chemistry Research Trends, Nova Science Publishers Inc., New York, 2009, pp. 265-287. [2] M. Masár, M. Zuborová, D. Kaniansky, B. Stanislawski, Determination of oxalate in beer by zone electrophoresis on a chip with conductivity detection, J. Sep. Sci. 26 (2003) 647-652. [3] Chutipongtanate S, Chaiyarit S, Thongboonkerd V. Citrate, not phosphate, can dissolve calcium oxalate monohydrate crystals and detach these crystals from renal tubular cells. Eur J Pharmacol 2012;689:219-25. [4] Weaver ML, Qiu SR, Hoyer JR, Casey WH, Nancollas GH, De Yoreo JJ

  8. Physical, chemical and radioactive characterization of co-products from titanium dioxide industry for valorization in the cement industry

    International Nuclear Information System (INIS)

    Gazquez, M.J.; Mantero, J.; Bolivar, J.P.; Garcia-Tenorio, R.; Vaca, F.

    2011-01-01

    The present study was conducted to characterize the raw materials (ilmenite and slag), waste (red gypsum) and several co-products (sulphate monohydrate and sulphate heptahydrated) form the titanium dioxide industry in relation to their elemental composition (major, minor and trace elements), granulometry, mineralogy, microscopic morphology, physical composition and radioactive content in order to apply this knowledge in the valorization of the co-products in the fields such a as construction, civil engineering, etc. In particular, the main properties of cements produced with different proportions of red gypsum were studied, and the obtained improvements, in relation to Ordinary Portland Cements (OPC) were evaluated. It was also demonstrated that the levels of pollutants and the radioactive content in the produced RG cements, remain within the regulated safety limits. (Author). 38 refs.

  9. Synthesis, characterization, and thermochemistry of the solid state coordination compound Zn(Nic){sub 2} . H{sub 2}O(s) (Nic = nicotinic acid)

    Energy Technology Data Exchange (ETDEWEB)

    Di Youying [College of Chemistry and Chemical Engineering, Liaocheng University, Liaocheng 252059, Shandong (China)], E-mail: yydi@lcu.edu.cn; Hong Yuanping; Kong Yuxia; Yang Weiwei [College of Chemistry and Chemical Engineering, Liaocheng University, Liaocheng 252059, Shandong (China); Tan Zhicheng [Thermochemistry Laboratory, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023 (China)

    2009-01-15

    A novel compound, viz. zinc nicotinate monohydrate, was synthesized by the method of room temperature solid phase synthesis. The techniques of FT-IR chemical and elemental analyses and X-ray powder diffraction were applied to characterise the structure and composition of the complex. In accordance with Hess' law, a thermochemical cycle was designed and the enthalpy change of the solid phase reaction of nicotinic acid with hydrated zinc acetate was determined to be {delta}{sub r}H{sub m}{sup 0}=(46.71{+-}0.21)kJ.mol{sup -1} by use of an isoperibol solution-reaction calorimeter. The standard molar enthalpy of formation of the title complex Zn(Nic){sub 2} . H{sub 2}O(s) was calculated as -(1062.3 {+-} 2.0) kJ . mol{sup -1} by use of the enthalpies of dissolution and other auxiliary thermodynamic data.

  10. DFT, FT-IR, FT-Raman and NMR studies of 4-(substituted phenylazo)-3,5-diacetamido-1H-pyrazoles

    Science.gov (United States)

    Kınalı, Selin; Demirci, Serkan; Çalışır, Zühre; Kurt, Mustafa; Ataç, Ahmet

    2011-05-01

    We present a detailed analysis of the structural and vibrational spectra of some novel azo dyes. 2-(Substituted phenylazo)malononitriles were synthesized by the coupling reaction of the diazonium salts, which were prepared with the use of various aniline derivatives with malononitrile, and then 4-(substituted phenylazo)-3,5-diamino-1H-pyrazole azo dyes were obtained via the ring closure of the azo compounds with hydrazine monohydrate. The experimental and theoretical vibrational spectra of azo dyes were studied. The structural and spectroscopic analysis of the molecules were carried out by using Becke's three-parameters hybrid functional (B3LYP) and density functional harmonic calculations. The 1H nuclear magnetic resonance (NMR) chemical shifts of the azo dye molecules were calculated using the gauge-invariant-atomic orbital (GIAO) method. The calculated vibrational wavenumbers and chemical shifts were compared with the experimental data of the molecules.

  11. Synthesis and characterization of novel benzohydrazide as potential antibacterial agents from natural product vanillin and wintergreen oil

    Science.gov (United States)

    Setyawati, Amri; Wahyuningsih, Tutik Dwi; Purwono, Bambang

    2017-03-01

    A chalcone-like benzohydrazide derivatives (3) has been synthesis from natural resources vanillin (1a) and wintergreen oil (1b). This compound was synthesis as modified natural resource antibacterial agent. Some modification was done to increase the biological activity. Bromide was introduced to the vanillin structure to increase the activity (2a), whereas Hydrazine monohydrate was reacted with wintergreen oil to make new nucleophile (2b). Furthermore, chalcone like benzohydrazide compound was synthesized by stirring 5-bromovanillin (2a) with salicyl hydrazine (2b) at room temperature for 2-3 hours. The product was analyzed by FTIR, GCMS, 1H- and 13C-NMR to confirm its structure. The result showed that 5-bromovanillin, salicyl hydrazine, and benzohydrazide were successfully synthesized with 98, 78, and 33% of yield respectively. The target molecule 3 achieved with yellowish color with m.p. 106-111 °C, 97% purity.

  12. Physical changes of beta-sitosterol crystals in oily suspensions during heating

    DEFF Research Database (Denmark)

    von Bonsdorff-Nikander, Anna; Lievonen, Satu; Christiansen, Leena

    2005-01-01

    with the mechanical properties of the suspensions during heating were studied by using variable temperature X-ray powder diffractometry (VT-XRPD), differential scanning calorimetry (DSC), and dynamic mechanical analysis (DMA). Hydrated beta-sitosterol crystals in an oil-suspension dehydrated, despite the composition...... of the suspensions, at low temperatures. At high beta-sitosterol concentration, the monohydrate crystal form changed partially to a hemihydrated form, and when only a small amount of water was initially incorporated, the hemihydrate crystal form dehydrated to a mostly anhydrate crystal form. The released water......, which was immiscible in the surrounding oil, caused the recrystallization of hydrated beta-sitosterol during cooling. This procedure indicated a reversible dehydration process. Structural and thermal analysis of beta-sitosterol crystals in suspensions, together with mechanical analysis made it possible...

  13. A second polymorph with composition Co3(PO42·H2O

    Directory of Open Access Journals (Sweden)

    Yang Kim

    2008-10-01

    Full Text Available Single crystals of Co3(PO42·H2O, tricobalt(II bis[orthophosphate(V] monohydrate, were obtained under hydrothermal conditions. The compound is the second polymorph of this composition and is isotypic with its zinc analogue, Zn3(PO42·H2O. Three independent Co2+ cations are bridged by two independent orthophosphate anions. Two of the metal cations exhibit a distorted tetrahedral coordination while the third exhibits a considerably distorted [5 + 1] octahedral coordination environment with one very long Co—O distance of 2.416 (3 Å. The former cations are bonded to four different phosphate anions, and the latter cation is bonded to four anions (one of which is bidentate and one water molecule, leading to a framework structure. Additional hydrogen bonds of the type O—H...O stabilize this arrangement.

  14. Urolithiasis associated with topiramate

    Directory of Open Access Journals (Sweden)

    Scott Eggener

    2004-02-01

    Full Text Available OBJECTIVE: Topiramate is a sulfamate-substituted monosaccharide anticonvulsant used as adjunctive therapy for intractable refractory seizures. It is report a case of topiramate-induced urolithiasis. CASE REPORT: A 35-year-old man presented with acute, right-sided, colicky flank pain. He denied hematuria or dysuria. He was in use of phenytoin, risperidone, phenobarbital, and topiramate. The total daily dose of topiramate was 375 mg. A CT scan showed a 7 x 1 mm curvilinear density at the right ureterovesical junction with proximal hydrouretronephrosis. He was managed with rigid ureteroscopic stone extraction and the calculus metabolic analysis revealed the stone was composed of carbonate apatite (70%, calcium oxalate dihydrate (20%, and calcium oxalate monohydrate (10%. COMMENTS: The present case typifies many features of topiramate-induced urolithiasis. Those who care for patients with urinary stone disease should be aware of this association.

  15. Kinetic concepts of thermally stimulated reactions in solids

    Science.gov (United States)

    Vyazovkin, Sergey

    Historical analysis suggests that the basic kinetic concepts of reactions in solids were inherited from homogeneous kinetics. These concepts rest upon the assumption of a single-step reaction that disagrees with the multiple-step nature of solid-state processes. The inadequate concepts inspire such unjustified anticipations of kinetic analysis as evaluating constant activation energy and/or deriving a single-step reaction mechanism for the overall process. A more adequate concept is that of the effective activation energy, which may vary with temperature and extent of conversion. The adequacy of this concept is illustrated by literature data as well as by experimental data on the thermal dehydration of calcium oxalate monohydrate and thermal decomposition of calcium carbonate, ammonium nitrate and 1,3,5,7- tetranitro-1,3,5,7-tetrazocine.

  16. Effective Nutritional Supplement Combinations

    Science.gov (United States)

    Cooke, Matt; Cribb, Paul J.

    Few supplement combinations that are marketed to athletes are supported by scientific evidence of their effectiveness. Quite often, under the rigor of scientific investigation, the patented combination fails to provide any greater benefit than a group given the active (generic) ingredient. The focus of this chapter is supplement combinations and dosing strategies that are effective at promoting an acute physiological response that may improve/enhance exercise performance or influence chronic adaptations desired from training. In recent years, there has been a particular focus on two nutritional ergogenic aids—creatine monohydrate and protein/amino acids—in combination with specific nutrients in an effort to augment or add to their already established independent ergogenic effects. These combinations and others are discussed in this chapter.

  17. Effect of medicinal plants on the crystallization of cholesterol

    Science.gov (United States)

    Saraswathi, N. T.; Gnanam, F. D.

    1997-08-01

    One of the least desirable calcifications in the human body is the mineral deposition in atherosclerosis plaques. These plaques principally consist of lipids such as cholesterol, cholesteryl esters, phospholipids and triglycerides. Chemical analysis of advanced plaques have shown the presence of considerable amounts of free cholesterol identified as cholesterol monohydrate crystals. Cholesterol has been crystallized in vitro. The extracts of some of the Indian medicinal plants detailed below were used as additives to study their effect on the crystallization behaviour of cholesterol. It has been found that many of the herbs have inhibitory effect on the crystallization such as nucleation, crystal size and habit modification. The inhibitory effect of the plants are graded as Commiphora mughul > Aegle marmeleos > Cynoden dactylon > Musa paradisiaca > Polygala javana > Alphinia officinarum > Solanum trilobatum > Enicostemma lyssopifolium.

  18. Imagine the Superiority of Dry Powder Inhalers from Carrier Engineering

    Directory of Open Access Journals (Sweden)

    Piyush Mehta

    2018-01-01

    Full Text Available Inhalation therapy has strong history of more than 4000 years and it is well recognized around the globe within every culture. In early days, inhalation therapy was designed for treatment of local disorders such as asthma and other pulmonary diseases. Almost all inhalation products composed a simple formulation of a carrier, usually α-lactose monohydrate orderly mixed with micronized therapeutic agent. Most of these formulations lacked satisfactory pulmonary deposition and dispersion. Thus, various alternative carrier’s molecules and powder processing techniques are increasingly investigated to achieve suitable aerodynamic performance. In view of this fact, more suitable and economic alternative carrier’s molecules with advanced formulation strategies are discussed in the present review. Furthermore, major advances, challenges, and the future perspective are discussed.

  19. Effects of pore shape and porosity on the properties of porous LNKN ceramics as bone substitute

    International Nuclear Information System (INIS)

    Wang Qi; Chen Qiang; Zhu Jianguo; Huang Chunpeng; Darvell, Brian W.; Chen Zhiqing

    2008-01-01

    A porous lead-free piezoelectric ceramic is investigated as direct bone substitute. Porous lithium sodium potassium niobate (Li 0.06 Na 0.5 K 0.44 )NbO 3 specimens were prepared by pore-forming method. Different volume fraction of ammonium oxalate monohydrate and poly(methyl methacrylate) were used as porogens to obtain different pore shape and porosity. Scanning electron microscopy showed a bicontinuous 3-3 structure of interconnected pores 150-250 μm in size. The piezoelectric constants and electromechanical coupling coefficients may be controlled by both size and shape of the porogens to tune for the best biological response. Such materials show promise for use as a piezoelectric composite bone substitute

  20. Near-infrared chemical imaging (NIR-CI) of 3D printed pharmaceuticals

    DEFF Research Database (Denmark)

    Khorasani, Milad; Edinger, Magnus; Raijada, Dharaben Kaushikkumar

    2016-01-01

    Hot-melt extrusion and 3D printing are enabling manufacturing approaches for patient-centred medicinal products. Hot-melt extrusion is a flexible and continuously operating technique which is a crucial part of a typical processing cycle of printed medicines. In this work we use hot-melt extrusion...... for manufacturing of medicinal films containing indomethacin (IND) and polycaprolactone (PCL), extruded strands with nitrofurantoin monohydrate (NFMH) and poly (ethylene oxide) (PEO), and feedstocks for 3D printed dosage forms with nitrofurantoin anhydrate (NFAH), hydroxyapatite (HA) and poly (lactic acid) (PLA......). These feedstocks were printed into a prototype solid dosage form using a desktop 3D printer. These model formulations were characterized using near-infrared chemical imaging (NIR-CI) and, more specifically, the image analytical data were analysed using multivariate curve resolution-alternating least squares (MCR...

  1. Tailored beads made of dissolved cellulose - Investigation of their drug release properties

    DEFF Research Database (Denmark)

    Yildir, Emrah; Kolakovic, Ruzica; Genina, Natalja

    2013-01-01

    In the frame of this work, we have investigated drug entrapping and release abilities of new type of porous cellulose beads (CBs) as a spherical matrix system for drug delivery. For that purpose, CBs prepared with three different methods were used as drug carriers and three compounds, anhydrous...... theophylline (Thp), riboflavin 5′-phosphate sodium (RSP) and lidocaine hydrochloride monohydrate (LiHCl) were used as model drug substances. The loading procedure was carried out by immersing swollen empty beads into the solutions of different concentrations of model drugs. The morphology of empty and loaded...... beads was examined using a field emission scanning electron microscopy (FE-SEM). Near-infrared (NIR) imaging was performed to identify the drug distributions on and within the loaded CBs. The drug amount incorporated into CBs was examined spectrophotometrically and in vitro drug release studies were...

  2. Effect of Zinc Methionine or Zinc Sulfate Supplementation on Milk Production and Composition of Milk in Lactating Dairy Cows

    DEFF Research Database (Denmark)

    Sobhanirad, Saeid; Carlson, Dorthe; Kashani, Reza Bahari

    2010-01-01

     Zn/kg of dry matter (DM) as zinc sulfate monohydrate (ZnS) and basal diet plus 500 mg Zn/kg of DM as zinc methionine (ZnM). Results showed that milk and fat-corrected milk yield in dairy cows were not significantly affected by Zn source although a numerical increase was observed. The percentages of protein......, lactose, fat, solid nonfat, total solid, and density of milk were not significantly different between treatments. However, dairy cows that received ZnM tended to produce more milk and fat-corrected milk with a lower somatic cell count as compared to controls. The zinc concentration in milk in the Zn...

  3. Effect of corrosion product layer on SCC susceptibility of copper containing type 304 stainless steel in 1 M H2SO4

    International Nuclear Information System (INIS)

    Asawa, M.; Devasenapathi, A.; Fujisawa, M.

    2004-01-01

    The effect of surface corrosion product layer on the stress corrosion cracking (SCC) susceptibility of type 304 stainless steel with Cu was studied in 1 kmol/m 3 (1 M) sulfuric acid at 353 K temperature. Studies based on the intermittent removal of surface corrosion product layer indicated that the surface film governs the SCC behavior of the alloy by accelerating both the crack initiation and propagation stages. The electrochemical impedance and polarization studies showed the surface layer to be promoting SCC initiation by lowering the uniform corrosion rate and the propagation by shifting the surface corrosion potential to a more noble direction. The elemental analysis of the corrosion product both by the energy dispersive X-ray (EDX) spectroscopy and by X-ray diffraction (XRD) analysis along with the thermodynamic calculations showed the layer to be constituted mainly of metallic copper (Cu) and the mono-hydrated iron sulfate which acts as cathode promoting SCC

  4. Continuous synthesis of Oleyl Oleate in supercritical carbon oxide using solid p-Toluenesulfonic Acid as catalyst

    International Nuclear Information System (INIS)

    Ghaziaskar, H.; Ikushima, Y.

    2000-01-01

    Supercritical carbon dioxide (Sc-CO 2 ) was used as solvent to synthesize oleyl oleate as an analog of Jojoba oil from oleic acid and oleyl alcohol with high conversion (100%) of the acid into ester in a short time of 100 min. Utilizing a low cost solid catalyst, p-toluenesulfonic acid monohydrate , the esterification reaction was performed, without any prior preparation step, in a flow mode, at a pressure of 147 bar and a temperature of 60 d eg C. This method seems industrially suitable for the production of oleyl oleate. The solubility of a mixture of oleyl alcohol and oleic acid in Sc-CO 2 were also measured to calculate the alcohol to acid ratio and the esterification yield

  5. Study of radial die-wall pressure changes during pharmaceutical powder compaction.

    Science.gov (United States)

    Abdel-Hamid, Sameh; Betz, Gabriele

    2011-04-01

    In tablet manufacturing, less attention is paid to the measurement of die-wall pressure than to force-displacement diagrams. Therefore, the aim of this study was to investigate radial stress change during pharmaceutical compaction. The Presster(TM), a tablet-press replicator, was used to characterize compaction behavior of microcrystalline cellulose (viscoelastic), calcium hydrogen phosphate dihydrate (brittle), direct compressible mannitol (plastic), pre-gelatinized starch (plastic/elastic), and spray dried lactose monohydrate (plastic/brittle) by measuring radial die-wall pressure; therefore powders were compacted at different (pre) compaction pressures as well as different speeds. Residual die-wall pressure (RDP) and maximum die-wall pressure (MDP) were measured. Various tablet physical properties were correlated to radial die-wall pressure. With increasing compaction pressure, RDP and MDP (P compaction behavior of materials and detecting friction phenomena in the early stage of development.

  6. Study of pertechnetate and perrhenate of calcium using infrared spectroscopy and PMR methods

    International Nuclear Information System (INIS)

    Teterin, Eh.G.; Zajtseva, L.L.; Samsonov, V.E.; Aksenenko, A.V.

    1986-01-01

    PMR and IR spectroscopic study of hydrates of calcium pertechnetate and perrhenates is carried out and their dehydration is studied. IR spectra analysis showed that dihydrates of calcium pertechnetate and perrhenate possess two types of crystal water molecules to which in spectra two sets of valence and deformation vibration bands and at least two types of pertechnetate and perrhenate groups correspond. During dehydration of calcium perrhenate dihydrate to monohydrate one type bond water molecules are withdrawn. The band set characteristic of the second type bond disappears only at complete dehydration of perrhenate, followed by spectrum simplification also in the region of perrhenate group absorption. Change of interproton distance in crystal water molecules under the action of crystal field, modifying during dehydration of calcium perrhenate dihydrate, is detected using PMR method

  7. Water-mediated tautomerization of cytosine to the rare imino form: An ab initio dynamics study

    Energy Technology Data Exchange (ETDEWEB)

    Fogarasi, Geza [Institute of Chemistry, Eotvos University, H-1518 Budapest, Pf. 32. (Hungary)], E-mail: fg@chem.elte.hu

    2008-06-16

    Tautomerism in nucleotide bases is one of the possible mechanisms of mutation of DNA. In spite of numerous studies on the structure and energy of cytosine tautomers, little information is available on the process of proton transfer itself. We present here Born-Oppenheimer dynamics calculations, with the potential surface obtained 'on the fly' from ab initio quantum chemistry (QC) and the atoms moving classically. In search for water-mediated tautomerization the monohydrated complex was studied, running about 300 trajectories each of 3000-5000 points of 1 fs steps. One single trajectory has been found to lead to tautomerization. Although the QC method used in the simulations was inevitably modest (B3LYP/3-21G), higher-level test calculations along the same trajectory suggest that the simulation grasped the basic mechanism of proton transfer: a concerted, synchronous process characterized by strong coupling between the motions of the two participating hydrogen atoms.

  8. AMP kinase expression and activity in human skeletal muscle: effects of immobilization, retraining, and creatine supplementation

    DEFF Research Database (Denmark)

    Eijnde, Bert O.; Derave, Wim; Wojtaszewski, Jørgen

    2005-01-01

    The effects of leg immobilization and retraining in combination with oral creatine intake on muscle AMP-activated protein kinase (AMPK) protein expression and phosphorylation status were investigated. A double-blind trial was performed in young healthy volunteers (n = 22). A cast immobilized...... the right leg for 2 wk, whereafter the knee-extensor muscles of that leg were retrained for 6 wk. Half of the subjects received creatine monohydrate throughout the study (Cr; from 15 g down to 2.5 g daily), and the others ingested placebo (P; maltodextrin). Before and after immobilization and retraining...... that immobilization-induced muscle inactivity for 2 wk does not alter AMPK a1-, a2-, and ß2-subunit expression or a-AMPK phosphorylation status. Furthermore, the present observations indicate that AMPK probably is not implicated in the previously reported beneficial effects of oral creatine supplementation on muscle...

  9. Small particle reagent based on crystal violet dye for developing latent fingerprints on non-porous wet surfaces

    Directory of Open Access Journals (Sweden)

    Richa Rohatgi

    2015-12-01

    Full Text Available Small particle reagent (SPR is a widely used method for developing latent fingerprints on non-porous wet surfaces. SPR based on zinc carbonate hydroxide monohydrate, ZnCo3·2Zn(OH2·H2O – also called basic zinc carbonate – has been formulated. The other ingredients of the formulation are crystal violet dye and a commercial liquid detergent. The composition develops clear, sharp and detailed fingerprints on non-porous items, after these were immersed separately in clean and dirty water for variable periods of time. The ability of the present formulation to detect weak and faint chance prints not only enhances its utility, but also its potentiality in forensic case work investigations. The raw materials used to prepare the SPR are cost-effective and non-hazardous.

  10. Synthesis of Ethane-1-Hydroxy-1,1-diphosphonic acid (EHDP) and preparation of labeled kits by 99mTc for bone studies

    International Nuclear Information System (INIS)

    Yassin, T.; Assaad, T.; Ghanem, E.; Ajaia, R.; Karajoli, N.

    2013-08-01

    Ethane-1-Hydroxy-1,1-diphosphonic acid monohydrate (EHDP) is very important precursor in radiopharmaceutical applications for bone diagnosis after labeling with 99mTc, was synthesized in high yield and purity. The compound was characterized by spectroscopic method. EHDP kit for bone imaging after labeling with technetium 99m was prepared according to an optimum conditions, Each vial contains 15 mg of EHDP and 25 mg of stannous chloride SnCl2. The prepared kit showed high quality satisfying the requirements of international pharmacopeias from of physical, chemical and radiochemical properties. The labeling yield exceeded 95% with an average value 99.6%. Biodistribution study of 99mTc-EHDP showed better clearance after three hours of injection in comparison with 99mTc-MDP kit (author).

  11. Comparative study on the predictability of statistical models (RSM and ANN) on the behavior of optimized buccoadhesive wafers containing Loratadine and their in vivo assessment.

    Science.gov (United States)

    Chakraborty, Prithviraj; Parcha, Versha; Chakraborty, Debarupa D; Ghosh, Amitava

    2016-01-01

    Buccoadhesive wafer dosage form containing Loratadine is formulated utilizing Formulation by Design (FbD) approach incorporating sodium alginate and lactose monohydrate as independent variable employing solvent casting method. The wafers were statistically optimized using Response Surface Methodology (RSM) and Artificial Neural Network algorithm (ANN) for predicting physicochemical and physico-mechanical properties of the wafers as responses. Morphologically wafers were tested using SEM. Quick disintegration of the samples was examined employing Optical Contact Angle (OCA). The comparison of the predictability of RSM and ANN showed a high prognostic capacity of RSM model over ANN model in forecasting mechanical and physicochemical properties of the wafers. The in vivo assessment of the optimized buccoadhesive wafer exhibits marked increase in bioavailability justifying the administration of Loratadine through buccal route, bypassing hepatic first pass metabolism.

  12. Attenuation measurements in solutions of some carbohydrates

    International Nuclear Information System (INIS)

    Gagandeep; Singh, K.; Lark, B.S.; Sahota, H.S.

    2000-01-01

    The linear attenuation coefficients in aqueous solutions of three carbohydrates, glucose (C 6 H 12 O 6 ), maltose monohydrate (C 12 H 22 O 11 ·H 2 O), and sucrose (C 12 H 22 O 11 ), were determined at 81, 356, 511, 662, 1,173, and 1,332 keV by the gamma-ray transmission method in a good geometry setup. From the precisely measured densities of these solutions, mass attenuation coefficients were then obtained that varied systematically with the corresponding changes in the concentrations (g/cm 3 ) of these solutions. The experimental results were used in terms of effective atomic numbers and electron densities. A comparison between experimental and theoretical values of attenuation coefficients has proven that the study has a potential application for the determination of attenuation coefficients of solid solutes from their solutions without obtaining them in pure crystalline form

  13. Attenuation Measurements in Solutions of Some Carbohydrates

    International Nuclear Information System (INIS)

    Gagandeep; Singh, Kulwant; Lark, B.S.; Sahota, H.S.

    2000-01-01

    The linear attenuation coefficients in aqueous solutions of three carbohydrates, glucose (C 6 H 12 O 6 ), maltose monohydrate (C 12 H 22 O 11 .H 2 O), and sucrose (C 12 H 22 O 11 ), were determined at 81, 356, 511, 662, 1173, and 1332 keV by the gamma-ray transmission method in a good geometry setup. From the precisely measured densities of these solutions, mass attenuation coefficients were then obtained that varied systematically with the corresponding changes in the concentrations (g/cm 3 ) of these solutions. The experimental results were used in terms of effective atomic numbers and electron densities. A comparison between experimental and theoretical values of attenuation coefficients has proven that the study has a potential application for the determination of attenuation coefficients of solid solutes from their solutions without obtaining them in pure crystalline form

  14. Thermal decomposition of RE(C2H5CO2)3·H2O (RE = Dy, Tb, Gd, Eu and Sm)

    DEFF Research Database (Denmark)

    Grivel, Jean-Claude

    2014-01-01

    The thermal decomposition of Dy(III), Tb(III), Gd(III), Eu(III), and Sm(III) propionate monohydrates was studied in argon by means of simultaneous differential thermal analysis and thermogravimetry, infrared-spectroscopy, X-ray diffraction, and optical microscopy. After dehydration, which takes......, an intermediate stage involving a RE2O(C2H5CO2)4 composition was evidenced in the case of the Eu- and Sm-propionates. For all compounds, further decomposition of RE2O2CO3 into the corresponding sesquioxides (RE2O3) is accompanied by the release of CO2. The thermal decomposition of Dy- and Tb-propionates occurs...

  15. A crude protective film on historic stones and its artificial preparation through biomimetic synthesis

    Science.gov (United States)

    Liu, Qiang; Zhang, Bingjian; Shen, Zhongyue; Lu, Huanming

    2006-12-01

    A biomimetic film has been found on the surface of the historic stone buildings and monuments. The stone inscriptions under the film are preserved so well that has not been damaged for more than 1000 years. Samples of the crude film have been analyzed by XRD, FTIR, PLM, EDA, SEM and TEM. The results show that it consists mainly of calcium oxalate monohydrate. On the basis of the existence of the organism debris, it is concluded that the film should be a product of biomineralization. According to this hypothesis, a similar film has been prepared on the stone surface through biomimetic synthesis in our laboratory. The preliminary analysis shows that the artificial protective film functions well.

  16. Molecular Complex of Lumiflavin and 2-Aminobenzoic Acid : Crystal Structure, Crystal Spectra, and Solution Properties

    OpenAIRE

    Shieh, Huey-Sheng; Ghisla, Sandro; Hanson, Louise Karle; Ludwig, Martha L.; Nordman, Christer E.

    1981-01-01

    The molecular complex lumiflavin-2-aminobenzoic acid monohydrate (C13H12N402●C7H7N02●H2O)crystallizes from aqueous solution as red triclinic prisms. The space group is P1 with cell dimensions a = 9.660 A, b = 14.866 Å, c = 7.045 Å, α = 95.44°, β = 95.86°, and γ = 105.66°. The crystal structure was solved by direct methods and refined by block-diagonal least-squares procedures to an R value of 0.050 on the basis of 1338 observed reflections. The structure is composed of stacks of alternating l...

  17. A terahertz transmission imaging based approach for liquid alcohol wettability investigation

    Science.gov (United States)

    Huang, Hui; Zhao, Hongwei; Zhang, Bo; Su, Yunyun; Jiang, Weixiang; Cai, Bin; You, Guanjun; Ma, Yan

    2018-03-01

    By using terahertz time-domain spectroscopy (THz-TDS), the transmission spectral images of a series of aliphatic monohydric liquid alcohols were investigated in this work. The image gray value indicated the non-uniform distribution of the liquid. After noise reduction, the depth distribution was computed from the image content, which depended on the wettability of the container surface by the liquid. Then the volume of the liquid crept up to the container surface was compared quantitatively. Our result showed that the surface wettability of the PS container surface by the liquids increased with the alcohol alkyl chain increasing, which was verified by the contact angle of the liquid and the surface. The study indicated that the THz image might offer a potential technique for detecting the wettability of liquid directly without an additional contact angle experiment.

  18. Characterisation of a novel transmission Raman spectroscopy platform for non-invasive detection of breast micro-calcifications

    Science.gov (United States)

    Ghita, Adrian; Matousek, Pavel; Stone, Nick

    2018-02-01

    Our work focuses on the development of a medical Raman spectroscopy based platform to non-invasively detect and determine in-vivo molecular information deep inside biological tissues by monitoring the chemical composition of breast calcifications. The ultimate goal is to replace a needle biopsy which typically follows the detection of an abnormality in mammographic images. Here we report the non-invasive detection of calcium oxalate monohydrate in tissue through 40 mm of phantom tissues using our recently developed advanced Raman instrument complementing our previous detection of calcium hydroxyapatite through this thickness of tissue. The ability to detect these two key types of calcifications opens avenues for the development of non-invasive in-vivo breast cancer diagnostic tool in the future.

  19. Semi-automatic determination of tin in marine materials by continuous flow hydride generation inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Feng Yonglai; Narasaki, Hisataki; Chen Hongyuan; Tian Liching

    1997-01-01

    A semi-automated continuous flow hydride generation system with inductively coupled plasma atomic emission spectrometry (ICP-AES) was used for the determination of tin in marine materials. The effects of acids (H 2 SO 4 and HCl) were studied. The analytical parameters were thoroughly investigated. Under optimized conditions, the detection limit is 0.4 ng/ml. Interferences from transition elements were investigated and seven masking reagents were tested. L-cysteine hydrochloride monohydrate (1%) was used to mask the interferences from foreign ions. Finally, the accuracy, checked with a marine standard reference material obtained from the National Research Council (NRC), was within the certified value. (orig.). With 6 figs., 4 tabs

  20. Preparation of calcium phosphate paste

    International Nuclear Information System (INIS)

    Mohd Reusmaazran Yusof; Norzita Yaacob; Idris Besar; Che Seman Mahmood; Rusnah Mustafa

    2010-01-01

    Calcium phosphate paste were prepared by mixing between calcium sodium potassium phosphate, Ca 2 NaK (PO 4 ) 2 (CSPP) and monocalcium phosphate monohydrate, Ca(H 2 PO 4 ) 2 .H 2 O (MCPM). CSPP were obtained by reaction between calcium hydrogen phosphate (CaHPO 4 ), potassium carbonate (K 2 CO 3 ) and sodium carbonate (Na 2 CO 3 ) in solid state sintering process followed by quenching in air at 1000 degree Celsius. The paste was aging in simulated body fluid (SBF) for 0.5, 1, 3, 6, 12, 24, 48 hrs, 3, 7 and 14 days. The morphological investigation indicated the formation of apatite crystal were first growth after 24 hours. The obvious growth of apatite crystal was shown at 3 days. The obvious growth of apatite crystal was shown in 7 and 14 days indicated the prediction of paste would have rapid reaction with bone after implantation. (author)

  1. Non-Traditional Systemic Treatments for Diabetic Retinopathy: An
Evidence-Based Review

    Science.gov (United States)

    Simó, Rafael; Ballarini, Stefania; Cunha-Vaz, José; Ji, Linong; Haller, Hermann; Zimmet, Paul; Wong, Tien Y.

    2015-01-01

    The rapid escalation in the global prevalence diabetes, with more than 30% being afflicted with diabetic retinopathy (DR), means it is likely that associated vision-threatening conditions will also rise substantially. This means that new therapeutic approaches need to be found that go beyond the current standards of diabetic care, and which are effective in the early stages of the disease. In recent decades several new pharmacological agents have been investigated for their effectiveness in preventing the appearance and progression of DR or in reversing DR; some with limited success while others appear promising. This up-to-date critical review of non-traditional systemic treatments for DR is based on the published evidence in MEDLINE spanning 1980-December 2014. It discusses a number of therapeutic options, paying particular attention to the mechanisms of action and the clinical evidence for the use of renin-angiotensin system blockade, fenofibrate and calcium dobesilate monohydrate in DR. PMID:25989912

  2. Effect of doxycycline vs placebo on retinal function and diabetic retinopathy progression in patients with severe nonproliferative or non-high-risk proliferative diabetic retinopathy

    DEFF Research Database (Denmark)

    Scott, Ingrid U; Jackson, Gregory R; Quillen, David A

    2014-01-01

    IMPORTANCE: Inflammation may contribute to the pathogenesis of diabetic retinopathy (DR). OBJECTIVES: To investigate, in a proof-of-concept clinical trial, whether low-dose oral doxycycline monohydrate can (1) slow the deterioration of, or improve, retinal function or (2) induce regression or slow......: We conducted a randomized, double-masked, 24-month proof-of-concept clinical trial. Thirty patients (from hospital-based retina practices) with 1 or more eyes with severe NPDR or PDR less than Early Treatment Diabetic Retinopathy Study-defined high-risk PDR. INTERVENTIONS: Patients were randomized...... adaptation, visual acuity, and quality of life) and anatomic factors (Early Treatment Diabetic Retinopathy Study DR severity level, area of retinal thickening, central macular thickness, macular volume, and retinal vessel diameters). RESULTS: From baseline to month 24, mean FDP foveal sensitivity decreased...

  3. New assignment of 14N NQR spectral lines for tetrazoles derivatives

    Science.gov (United States)

    Mamadazizov, Sultonazar; Shelyapina, Marina G.; Kupriyanova, Galina S.; Mozzhukhin, George V.

    2018-04-01

    In recent years, considerable interest has been shown in the study of tetrazole derivatives, which attract attention as highly nitrogenous compounds for use as an isosteric substitutes for various functional groups that leads to creation of novel biologically active substances. NQR techniques, being sensitive to the local environment of 14N nuclei, provide great opportunities to study these new substances. To make investigation of complex compounds containing tetrazoles derivatives easier and more reliable a correctly assigned 14N NQR spectra of tetrazoles are required. Here we report on the results of our DFT B3LYP calculations of 14N NQR spectral parameters (quadrupole coupling constant Qcc and the asymmetry parameter of the electric field gradient η) for tetrazole, 5-aminotetrazole and 5-aminotetrazole monohydrate. It has been found that the commonly accepted assignment of the 14N NQR spectral lines for these molecules is incorrect. A new assignment for these molecules is proposed.

  4. Wetting effect on optical sum frequency generation (SFG) spectra of D-glucose, D-fructose, and sucrose

    Science.gov (United States)

    Hieu, Hoang Chi; Li, Hongyan; Miyauchi, Yoshihiro; Mizutani, Goro; Fujita, Naoko; Nakamura, Yasunori

    2015-03-01

    We report a sum frequency generation (SFG) spectroscopy study of D-glucose, D-fructose and sucrose in the Csbnd H stretching vibration regime. Wetting effect on the SFG spectra was investigated. The SFG spectrum of D-glucose changed from that of α-D-glucose into those of α-D-glucose monohydrate by wetting. The SFG spectra showed evidence of a small change of β-D-fructopyranose into other anomers by wetting. SFG spectra of sucrose did not change by wetting. Assignments of the vibrational peaks in the SFG spectra of the three sugars in the dry and wet states were performed in the Csbnd H stretching vibration region near 3000 cm-1.

  5. Nuclear magnetic resonance studies of ion motion in solid electrolytes. Annual report, June 1, 1982-March 31, 1983

    International Nuclear Information System (INIS)

    Bjorkstam, J.L.

    1983-01-01

    An extensive investigation of a number of Li-Na beta-alumina crystals was carried out. It was found that the reaction of beta-aluminas with water involves partial substitution of M + by H 3 O + (or H + ) and carbonation at the crystal surface; i.e., reaction of a hydroxide with CO 2 . NMR spin-lattice relaxation data have been collected over the 4.2-100 0 K temperature interval at several frequencies for a number of beta-aluminas. Extensive efforts on the NMR investigation of lithium, proton, and deuteron nuclei in both normal and deuterated single crystals of lithium-iodide-monohydrate are reported. An extensive investigation of the thermodynamics and cation exchange properties of the AgI: Ag 2 O-B 2 O 3 glasses has been performed. Cation exchange techniques to produce new vitreous electrolytes were not successful

  6. Reaction between drug substances and pharmaceutical excipients

    DEFF Research Database (Denmark)

    Larsen, Jesper; Cornett, Claus; Jaroszewski, Jerzy Witold

    2009-01-01

    The reactivity of citric acid towards drug substances in the solid state was examined using the beta-blocker carvedilol as a model compound. The reaction mixtures were analysed by LC-MS, the reaction products were isolated by preparative HPLC, and the structures were elucidated by microprobe NMR...... spectroscopy. Heating a mixture of solid carvedilol and solid citric acid monohydrate for 96h at 50 degrees C resulted in the formation of about 3% of a symmetrical ester as well as of a number of other reaction products in smaller amounts. Formation of the symmetrical ester was also observed at room...... temperature. At 70 degrees C, the amounts of three isomeric esters formed reached 6-8%. The minor reaction products were citric acid amides, O-acetylcarvedilol, and esters of itaconic acid....

  7. Renal geology (quantitative renal stone analysis) by 'Fourier transform infrared spectroscopy'.

    Science.gov (United States)

    Singh, Iqbal

    2008-01-01

    To prospectively determine the precise stone composition (quantitative analysis) by using infrared spectroscopy in patients with urinary stone disease presenting to our clinic. To determine an ideal method for stone analysis suitable for use in a clinical setting. After routine and a detailed metabolic workup of all patients of urolithiasis, stone samples of 50 patients of urolithiasis satisfying the entry criteria were subjected to the Fourier transform infrared spectroscopic analysis after adequate sample homogenization at a single testing center. Calcium oxalate monohydrate and dihydrate stone mixture was most commonly encountered in 35 (71%) followed by calcium phosphate, carbonate apatite, magnesium ammonium hexahydrate and xanthine stones. Fourier transform infrared spectroscopy allows an accurate, reliable quantitative method of stone analysis. It also helps in maintaining a computerized large reference library. Knowledge of precise stone composition may allow the institution of appropriate prophylactic therapy despite the absence of any detectable metabolic abnormalities. This may prevent and or delay stone recurrence.

  8. Sibutramine, a serotonin-norepinephrine reuptake inhibitor, causes fibrosis in rats.

    Science.gov (United States)

    Oberholzer, Hester Magdalena; van der Schoor, Ciska; Bester, Megan Jean

    2015-07-01

    Sibutramine hydrochloride monohydrate is a weight loss agent indicated for the treatment of obesity. Although it has been banned from most markets, studies are still relevant as it is often a hidden ingredient in herbal and over the counter slimming products. Sibutramine induces liver fibrosis with steatosis in female Sprague-Dawley rats fed a high-energy diet without significant weight gain. In this study, using the same animal model, the effect of Sibutramine on lung morphology was investigated using histological evaluation of the terminal bronchiole and transmission electron microscopy evaluation of the respiratory tissue. From these results Sibutramine was found to induce lung fibrosis in Sprague-Dawley rats as increased collagen synthesis, mast cell accumulation and aggregates of Bronchus Associated Lymphoid Tissue (BALT) in the terminal bronchiole as well as increased collagen deposition in the respiratory tissue was seen. Copyright © 2015 Elsevier B.V. All rights reserved.

  9. Sibutramine selective electrodes for batch and flow injection determinations in pharmaceutical preparations.

    Science.gov (United States)

    Zayed, S I M; Issa, Y M

    2010-01-01

    The construction and electrochemical response characteristics of two new polyvinyl chloride (PVC) membrane sensors for the determination of sibutramine hydrochloride were described. The sensors are based on the ion association complexes of sibutramine with sodium tetraphenylborate (NaTPB) or phosphotungstic acid (PTA) using dibutyl phthalate as plasticizing solvent. The sensors display a fast, stable response over the concentration range 3.84 x 10(-5)-1.00 x 10(-2) M sibutramine hydrochloride monohydrate (SibuCl), with cationic slopes of 57.7 +/- 0.57 and 59.7 +/- 1.79 mV concentration decade(-1) and detection limits of 8.91 x 10(-6) and 1.47 x 10(-5) M in case of sibutramine-tetraphenylborate (Sibu-TPB) and sibutramine-phosphotungstate ((Sibu)(3)-PT), respectively. The proposed sensors have been successfully applied for the determination of sibutramine hydrochloride in Regitrim capsules in batch and flow injection (FI) conditions.

  10. Physical, chemical and radioactive characterization of co-products from titanum dioxide industry for valorization in the cement industry; Caracterizacion fisico-quimica y radiactiva de los sub-productos provenientes de la industria de dioxido de titanio para su valorizacion en la industria del cemento: implicaciones radiologicas.

    Energy Technology Data Exchange (ETDEWEB)

    Gazquez, M.J.; Mantero, J.; Bolivar, J.P.; Garcia-Tenorio, R.; Vaca, F.

    2011-07-01

    The present study was conducted to characterize the raw materials (ilmenite and slag), waste (red gypsum) and several co-products (sulphate monohydrate and sulphate heptahydrated) form the titanum dioxide industry in relation to their elemental composition (major, minor and trace elements), granulometry, mineralogy, microscopic morphology, physical composition and radioactive content in order to apply this knowledge in the valorization of the co-products in the fields sucha as construction, civil engineering, etc. In particular, the main properties of cements produced with different proportions of red gypsum were studied, and the obtained improvements, in relation to Ordinary Portland Cements (OPC) were evaluated. It was also demonstrated that the levels of pollutants and the radioactive content in the produced RG cements, remain within the regulated safety limits. (Author). 38 refs.

  11. Physical, chemical and radioactive characterization of co-products from titanium dioxide industry for valorization in the cement industry; Caracterizacion fisico-quimica y radiactiva de los sub-productos provenientes de la industria de dioxido de titanio para su valorizacion en la industria del cemento: implicaciones radiologicas.

    Energy Technology Data Exchange (ETDEWEB)

    Gazquez, M.J.; Mantero, J.; Bolivar, J.P.; Garcia-Tenorio, R.; Vaca, F.

    2011-07-01

    The present study was conducted to characterize the raw materials (ilmenite and slag), waste (red gypsum) and several co-products (sulphate monohydrate and sulphate heptahydrated) form the titanium dioxide industry in relation to their elemental composition (major, minor and trace elements), granulometry, mineralogy, microscopic morphology, physical composition and radioactive content in order to apply this knowledge in the valorization of the co-products in the fields such a as construction, civil engineering, etc. In particular, the main properties of cements produced with different proportions of red gypsum were studied, and the obtained improvements, in relation to Ordinary Portland Cements (OPC) were evaluated. It was also demonstrated that the levels of pollutants and the radioactive content in the produced RG cements, remain within the regulated safety limits. (Author). 38 refs.

  12. Creatine-induced activation of antioxidative defence in myotube cultures revealed by explorative NMR-based metabonomics and proteomics

    DEFF Research Database (Denmark)

    Young, Jette Feveile; Larsen, Lotte Bach; Malmendal, Anders

    2010-01-01

    Creatine is a key intermediate in energy metabolism and supplementation of creatine has been used for increasing muscle mass, strength and endurance. Creatine supplementation has also been reported to trigger the skeletal muscle expression of insulin like growth factor I, to increase the fat......-free mass and improve cognition in elderly, and more explorative approaches like transcriptomics has revealed additional information. The aim of the present study was to reveal additional insight into the biochemical effects of creatine supplementation at the protein and metabolite level by integrating...... the explorative techniques, proteomics and NMR metabonomics, in a systems biology approach. METHODS: Differentiated mouse myotube cultures (C2C12) were exposed to 5 mM creatine monohydrate (CMH) for 24 hours. For proteomics studies, lysed myotubes were analyzed in single 2-DGE gels where the first dimension...

  13. Hepatoprotective and Hypolipidemic Effects of Carthamus tinctorius oil in Alloxan-induced Type 1 Diabetic Rats

    Directory of Open Access Journals (Sweden)

    Rahimi Parivash

    2014-04-01

    Full Text Available Introduction: Hepatoprotective and hypolipidemic effects of Carthamus tinctorius Linn.(Safflower seed oil was investigated in diabetic rats. Methods: Diabetes was induced by administration of 120 mg/kg alloxan monohydrate. The seed oil of safflower at dose of 200 mg/kg was administered as single dose per day to diabetic rats for a period of 28 days. The effect of oil on blood glucose level was measured in the diabetic rats. Serum lipid profile [total cholesterol (TC, triglycerides (TGs, low density (LDL and high density lipoprotein (HDL and enzymes such as alanine aminotransferase (ALT, aspartate aminotransferase (AST and alkaline phosphatase (ALP were also determined. Results: Levels of blood glucose, TC, TGs, LDL, ALT, AST and ALP decreased and HDL increased in alloxan induced diabetic rats after treatment with 200 mg/kg safflower seed oil for 28 days. Conclusion: The present study demonstrates that seed oil of safflower seems to be useful for the prevention of diabetes complications.

  14. Effective modification of particle surface properties using ultrasonic water mist

    DEFF Research Database (Denmark)

    Genina, Natalja; Räikkönen, Heikki; Heinämäki, Jyrki

    2009-01-01

    The goal of the present study was to design a new technique to modify particle surface properties and, through that, to improve flowability of poorly flowing drug thiamine hydrochloride and pharmaceutical sugar lactose monohydrate of two different grades. The powdered particles were supplied...... properties. It was found that rapid exposition of pharmaceutical materials by water mist resulted in the improvement of powder technical properties. The evident changes in flowability of coarser lactose were obviously due to smoothing of particle surface and decreasing in the level of fines with very slight...... increment in particle size. The changes in thiamine powder flow were mainly due to narrowing in particle size distribution where the tendency for better flow of finer lactose was related to surface and size modifications. The aqueous mist application did not cause any alteration of the crystal structures...

  15. Comparison of torque measurements and near-infrared spectroscopy in characterization of a wet granulation process

    DEFF Research Database (Denmark)

    Jørgensen, Anna Cecilia; Luukkonen, Pirjo; Rantanen, Jukka

    2004-01-01

    The purpose of this study was to compare impeller torque measurements and near-infrared (NIR) spectroscopy in the characterization of the water addition phase of a wet granulation process. Additionally, the effect of hydrate formation during granulation on the impeller torque was investigated....... Anhydrous theophylline, alpha-lactose monohydrate, and microcrystalline cellulose (MCC) were used as materials for the study. The materials and mixtures of them were granulated using purified water in a small-scale high-shear mixer. The impeller torque was registered and NIR spectra of wet samples were...... recorded at-line. The torque and the NIR baseline-corrected water absorbances increased with increasing water content. A plateau in the NIR baseline-corrected water absorbances was observed for wet masses containing MCC. This was at the region of optimal water amount for granulation according to the torque...

  16. IUPAC-NIST Solubility Data Series. 95. Alkaline Earth Carbonates in Aqueous Systems. Part 2. Ca

    Science.gov (United States)

    Vanderdeelen, Jan

    2012-06-01

    The alkaline earth carbonates are an important class of minerals. This article is part of a volume in the IUPAC-NIST Solubility Data Series that compiles and critically evaluates solubility data of the alkaline earth carbonates in water and in simple aqueous electrolyte solutions. Part 1 outlined the procedure adopted in this volume, and presented the beryllium and magnesium carbonates. Part 2, the current paper, compiles and critically evaluates the solubility data of calcium carbonate. The chemical forms included are the anhydrous CaCO3 types calcite, aragonite, and vaterite, the monohydrate monohydrocalcite (CaCO3. H2O), the hexahydrate ikaite (CaCO3.6H2O), and an amorphous form. The data were analyzed with two model variants, and thermodynamic data of each form consistent with each of the models and with the CODATA key values for thermodynamics are presented.

  17. IUPAC-NIST Solubility Data Series. 95. Alkaline Earth Carbonates in Aqueous Systems. Part 2. Ca

    International Nuclear Information System (INIS)

    De Visscher, Alex; Vanderdeelen, Jan

    2012-01-01

    The alkaline earth carbonates are an important class of minerals. This article is part of a volume in the IUPAC-NIST Solubility Data Series that compiles and critically evaluates solubility data of the alkaline earth carbonates in water and in simple aqueous electrolyte solutions. Part 1 outlined the procedure adopted in this volume, and presented the beryllium and magnesium carbonates. Part 2, the current paper, compiles and critically evaluates the solubility data of calcium carbonate. The chemical forms included are the anhydrous CaCO 3 types calcite, aragonite, and vaterite, the monohydrate monohydrocalcite (CaCO 3 · H 2 O), the hexahydrate ikaite (CaCO 3 ·6H 2 O), and an amorphous form. The data were analyzed with two model variants, and thermodynamic data of each form consistent with each of the models and with the CODATA key values for thermodynamics are presented.

  18. IUPAC-NIST Solubility Data Series. 95. Alkaline Earth Carbonates in Aqueous Systems. Part 2. Ca

    Energy Technology Data Exchange (ETDEWEB)

    De Visscher, Alex; Vanderdeelen, Jan [Department of Chemical and Petroleum Engineering, and Centre for Environmental Engineering Research and Education (CEERE), Schulich School of Engineering, University of Calgary, Calgary, Alberta, T2N 1N4 (Canada); Department of Applied Analytical and Physical Chemistry, Faculty of Bioscience Engineering, Ghent University, B-9000 Ghent (Belgium)

    2012-06-15

    The alkaline earth carbonates are an important class of minerals. This article is part of a volume in the IUPAC-NIST Solubility Data Series that compiles and critically evaluates solubility data of the alkaline earth carbonates in water and in simple aqueous electrolyte solutions. Part 1 outlined the procedure adopted in this volume, and presented the beryllium and magnesium carbonates. Part 2, the current paper, compiles and critically evaluates the solubility data of calcium carbonate. The chemical forms included are the anhydrous CaCO{sub 3} types calcite, aragonite, and vaterite, the monohydrate monohydrocalcite (CaCO{sub 3}{center_dot} H{sub 2}O), the hexahydrate ikaite (CaCO{sub 3}{center_dot}6H{sub 2}O), and an amorphous form. The data were analyzed with two model variants, and thermodynamic data of each form consistent with each of the models and with the CODATA key values for thermodynamics are presented.

  19. Solid state conformations and antidopaminergic effects of remoxipride hydrochloride and a closely related salicylamide, FLA 797, in relation to dopamine receptor models.

    Science.gov (United States)

    Högberg, T; Rämsby, S; de Paulis, T; Stensland, B; Csöregh, I; Wägner, A

    1986-10-01

    The X-ray structures of two new 2,6-disubstituted benzamides, i.e., remoxipride hydrochloride monohydrate [-)-(S)-3-bromo-N-[(1-ethyl-2-pyrrolidinyl)methyl]-2,6-dimethoxybenza mide hydrochloride monohydrate) and FLA 797 [-)-(S)-3-bromo-N-[(1-ethyl-2-pyrrolidinyl)methyl]-6-methoxysalicylamide ), have been determined as well as the distribution coefficients. The difference in dopamine receptor blocking activity is discussed in terms of lipophilicity and solid state conformations of the two benzamides. The major difference between the solid state conformations lies in the orientation of the carboxamide moiety. In remoxipride the carbonyl group is oriented almost perpendicularly to the benzene ring, thus preventing the formation of a hydrogen-bonded pseudo-ring between the amide hydrogen and the methoxy group found in other types of o-methoxybenzamides. In FLA 797, however, this pseudo-ring is present in the planar conformation of the salicylamide moiety. This conformation is further stabilized by a hydrogen bond between the phenol group and the carbonyl oxygen. The side chain in remoxipride adopts an extended conformation in contrast to FLA 797, where the side chain has a folded conformation. The crystal structures are related to current topographic dopamine receptor models developed from more rigid antidopaminergic compounds. Based on these comparisons, it is suggested that benzamides having an N-ethyl-2-pyrrolidinylmethyl side chain interact with the receptor in the folded conformation. The binding affinity is thought to be further increased by the planar conformation of the salicylamide moiety present in FLA 797, which permits an efficient pi-pi stacking interaction.

  20. Supramolecular Organization of Nonstoichiometric Drug Hydrates: Dapsone

    Directory of Open Access Journals (Sweden)

    Doris E. Braun

    2018-02-01

    Full Text Available The observed moisture- and temperature dependent transformations of the dapsone (4,4′-diaminodiphenyl sulfone, DDS 0. 33-hydrate were correlated to its structure and the number and strength of the water-DDS intermolecular interactions. A combination of characterization techniques was used, including thermal analysis (hot-stage microscopy, differential scanning calorimetry and thermogravimetric analysis, gravimetric moisture sorption/desorption studies and variable humidity powder X-ray diffraction, along with computational modeling (crystal structure prediction and pair-wise intermolecular energy calculations. Depending on the relative humidity the hydrate contains between 0 and 0.33 molecules of water per molecule DDS. The crystal structure is retained upon dehydration indicating that DDS hydrate shows a non-stoichiometric (dehydration behavior. Unexpectedly, the water molecules are not located in structural channels but at isolated-sites of the host framework, which is counterintuitively for a hydrate with non-stoichiometric behavior. The water-DDS interactions were estimated to be weaker than water-host interactions that are commonly observed in stoichiometric hydrates and the lattice energies of the isomorphic dehydration product (hydrate structure without water molecules and (form III differ only by ~1 kJ mol−1. The computational generation of hypothetical monohydrates confirms that the hydrate with the unusual DDS:water ratio of 3:1 is more stable than a feasible monohydrate structure. Overall, this study highlights that a deeper understanding of the formation of hydrates with non-stoichiometric behavior requires a multidisciplinary approach including suitable experimental and computational methods providing a firm basis for the development and manufacturing of high quality drug products.