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Sample records for compound uru2si2 determined

  1. Electrical transport in URu2Si2

    International Nuclear Information System (INIS)

    Dawson, A.LeR.; Datars, W.R.; Garrett, J.D.; Razavi, F.S.

    1989-01-01

    The temperature dependence of the resistivity, magnetic susceptibility and Hall coefficient have been measured in oriented single-crystals of URu 2 Si 2 . The susceptibility is Curie-Weiss like at high temperatures and the anisotropy shows that the f moments on the U atoms are highly confined to lie along the c direction. The resistivity is analysed in terms of a Kondo-like behaviour at high temperatures and shows the onset of coherence, modified by electron-spin wave scattering, at low temperatures. There is a sharp superconducting transition at 1.33 K. The Hall coefficient is analysed by using a modification of the recent theory by Fert and Levy and suggests that the coherence temperature T 0 and the Kondo temperature T k need not be sharply distinguished in URu 2 Si 2 . There is a large increase in the Hall coefficient as the temperature is lowered below 18 K which is attributed to a Fermi surface restructuring, possibly due to the existence of spin density waves in the antiferromagnetic state. (author)

  2. Implications of the measured angular anisotropy at the hidden order transition of URu2Si2

    Science.gov (United States)

    Chandra, P.; Coleman, P.; Flint, R.; Trinh, J.; Ramirez, A. P.

    2018-05-01

    The heavy fermion compound URu2Si2 continues to attract great interest due to the long-unidentified nature of the hidden order that develops below 17.5 K. Here we discuss the implications of an angular survey of the linear and nonlinear susceptibility of URu2Si2 in the vicinity of the hidden order transition [1]. While the anisotropic nature of spin fluctuations and low-temperature quasiparticles was previously established, our recent results suggest that the order parameter itself has intrinsic Ising anisotropy, and that moreover this anisotropy extends far above the hidden order transition. Consistency checks and subsequent questions for future experimental and theoretical studies of hidden order are discussed.

  3. Origin of the exceptional Ising behavior of quasiparticles in the hiddenorder material URu2Si2

    International Nuclear Information System (INIS)

    Werwinski, Miroslaw; Rusz, Jan; Oppeneer, Peter M.; Mydosh, John A.

    2014-01-01

    The hidden order (HO) phase emerging below 17.5K in the heavy-fermion compound URu2Si2 has drawn considerable attention. In spite of intensive experimental and theoretical investigations the origin of the arising electronic order could not be unambiguously explained. Multifarious theories have been proposed to explain the intriguing appearance of the HO phase [1]. Since the actinide 5f electrons can adopt localized or itinerant character, theories based on localized 5f behavior have been proposed as well as competing theories based on the assumption of itinerant 5f behavior; in the latter the existence of a Fermi surface instability is central

  4. Hidden order and disorder effects in URu2Si2

    Science.gov (United States)

    Bernal, O. O.; Moroz, M. E.; Ishida, K.; Murakawa, H.; Reyes, A. P.; Kuhns, P. L.; MacLaughlin, D. E.; Mydosh, J. A.; Gortenmulder, T. J.

    2006-05-01

    NMR experiments at ambient pressure in URu 2Si 2 demonstrate a linewidth enhancement effect below the hidden order transition temperature T0. We present single-crystal 29Si NMR parameters for various temperatures and for an applied magnetic field perpendicular to the crystal c-axis. By comparing oriented-powder and single-crystal data, we observe that the size of the linewidth enhancement below T0 correlates with the size of the high- T broadening. We measure a 29Si up-field line shift below T0 which indicates the presence of an internal-field average for the entire crystal. This shift also correlates with the high-temperature width. The 101Ru NQR frequency as a function of temperature was also measured. No strong effect on the NQR frequency is observed at T0. Both NMR and NQR measurements suggest a connection between linewidth/disorder effects and the transition to hidden order.

  5. Magnetic excitations in the heavy-Fermion superconductor URu2Si2

    DEFF Research Database (Denmark)

    Broholm, C.; Lin, H.; Matthews, P.T.

    1991-01-01

    Antiferromagnetic order and fluctuations in the heavy-fermion superconductor URu2Si2 have been studied by magnetic neutron scattering. Below T(N) = 17.5 K, URu2Si2 is a type-I antiferromagnet with an anomalously small ordered moment of (0.04 +/- 0.01)mu-B polarized along the tetragonal c axis...

  6. Translational Symmetry Breaking and Gapping of Heavy-Quasiparticle Pocket in URu2Si2

    Science.gov (United States)

    Yoshida, Rikiya; Tsubota, Koji; Ishiga, Toshihiko; Sunagawa, Masanori; Sonoyama, Jyunki; Aoki, Dai; Flouquet, Jacques; Wakita, Takanori; Muraoka, Yuji; Yokoya, Takayoshi

    2013-01-01

    URu2Si2 is a uranium compound that exhibits a so-called ‘hidden-order’ transition at ~17.5 K. However, the order parameter of this second-order transition as well as many of its microscopic properties remain unclarified despite considerable research. One of the key questions in this regard concerns the type of spontaneous symmetry breaking occurring at the transition; although rotational symmetry breaking has been detected, it is not clear whether another type of symmetry breaking also occurs. Another key question concerns the property of Fermi-surface gapping in the momentum space. Here we address these key questions by a momentum-dependent observation of electronic states at the transition employing ultrahigh-resolution three-dimensional angle-resolved photoemission spectroscopy. Our results provide compelling evidence of the spontaneous breaking of the lattice's translational symmetry and particle-hole asymmetric gapping of a heavy quasiparticle pocket at the transition. PMID:24084937

  7. Competition of ground states in URu2Si2 and UCoGe

    International Nuclear Information System (INIS)

    Hassinger, E.

    2010-10-01

    In this thesis, two uranium based heavy fermion compounds are studied under pressure. URu2Si2 has a mysterious ground state below T0 = 17.5 K at ambient pressure. The order parameter has not been identified yet which led to the name 'hidden order' (HO). In addition, below 1.5 K the system becomes superconducting. With pressure, the ground state switches from the HO phase to an antiferromagnetic (AF) phase at a critical pressure and superconductivity is concomitantly suppressed. Shubnikov-de Haas measurements under pressure show that the Fermi surface doesn't change between the two phases. The folding of the Fermi surface which occurs in the high pressure AF phase therefore already happens in the HO phase, indicating a unit cell doubling. Our measurements of the complete angular dependence of the oscillation frequencies test the electronic structure and support new theoretical band structure calculations with rather itinerant 5f electrons. The second part of my research focuses on another uranium compound, UCoGe. It is one of the few known materials where superconductivity (Tsc = 0.6 K) coexists with ferromagnetism (T Curie = 2.8 K). Precise studies of the pressure phase diagram by resistivity, ac calorimetry and ac susceptibility show that the ferromagnetic phase is suppressed at a pressure of about 1 GPa and the superconducting phase extends into the paramagnetic phase induced by pressure. When ferromagnetism is suppressed to the superconducting transition no further distinct ferromagnetic anomalies are observed. Thus, the pressure phase diagram of UCoGe is unique in the class of ferromagnetic superconductors. (author)

  8. Theoretical reconsideration of antiferromagnetic Fermi surfaces in URu2Si2

    International Nuclear Information System (INIS)

    Yamagami, Hiroshi

    2011-01-01

    In an itinerant 5f-band model, the antiferromagnetic (AFM) Fermi surfaces of URu 2 Si 2 are reconsidered using a relativistic LAPW method within a local spin-density approximation, especially taking into account the lattice parameters dependent on pressures. The reduction of the z-coordinate of the Si sites results in the effect of flattening the Ru-Si layers of URu 2 Si 2 crystal structure, thus weakening a hybridization/mixing between the U-5f and Ru-4d states in the band structure. Consequently the 5f bands around the Fermi level are more flat in the dispersion with decreasing the z-coordinate, thus producing three closed Fermi surfaces like 'curing-stone', 'rugby-ball' and 'ball'. The origins of de Haas-van Alphen branches can be qualitatively interpreted from the obtained AFM Fermi surfaces.

  9. A model for metastable magnetism in the hidden-order phase of URu2Si2

    Science.gov (United States)

    Boyer, Lance; Yakovenko, Victor M.

    2018-01-01

    We propose an explanation for the experiment by Schemm et al. (2015) where the polar Kerr effect (PKE), indicating time-reversal symmetry (TRS) breaking, was observed in the hidden-order (HO) phase of URu2Si2. The PKE signal on warmup was seen only if a training magnetic field was present on cool-down. Using a Ginzburg-Landau model for a complex order parameter, we show that the system can have a metastable ferromagnetic state producing the PKE, even if the HO ground state respects TRS. We predict that a strong reversed magnetic field should reset the PKE to zero.

  10. Thermodynamic aspect in using modified Boltzmann model as an acoustic probe for URu2Si2

    Science.gov (United States)

    Kwang-Hua, Chu Rainer

    2018-05-01

    The approximate system of equations describing ultrasonic attenuation propagating in many electrons of the heavy-fermion materials URu2Si2 under high magnetic fields were firstly derived and then calculated based on the modified Boltzmann model considering the microscopic contributions due to electronic fluids. A system of nonlinear partial differential coupled with integral equations were linearized firstly and approximately solved considering the perturbed thermodynamic equilibrium states. Our numerical data were compared with previous measurements using non-dimensional or normalized physical values. The rather good fit of our numerical calculations with experimental measurements confirms our present approach.

  11. Magnetic Correlations in URu2Si2 under Chemical and Hydrostatic Pressure

    Science.gov (United States)

    Williams, Travis; Aczel, Adam; Broholm, Collin; Buyers, William; Leao, Juscelino; Luke, Graeme; Rodriguez-Riviera, Jose; Stone, Matthew; Wilson, Murray; Yamani, Zahra

    URu2Si2 has been an intense area of study for the last 30 years due to a mysterious hidden order phase that appears below T0 = 17.5 K. The hidden order phase has been shown to be extremely sensitive to perturbations, being destroyed quickly by the application of a magnetic field, hydrostatic or uniaxial pressure, and chemical doping. While attempting to understand the properties of URu2Si2, neutron scattering has found spin correlations that are intimately related to this hidden order phase and which are also suppressed with these perturbations. Here, I will outline some recent neutron scattering work to study these correlations in two exceptional cases where the hidden order phase is enhanced: hydrostatic pressure and chemical pressure using Fe- and Os-doping. In both of these cases, T0 increases before an antiferromagnetic phase emerges. By performing a careful analysis of the neutron data, we show that these two phases are much more related than had been previously appreciated. This implies that the hidden order is likely compatible with an antiferromagnetic ground state, placing constraints on the nature of the missing order parameter.

  12. Partially gapped Fermi surface in the heavy-electron superconductor URu2Si2

    International Nuclear Information System (INIS)

    Maple, M.B.; Chen, J.W.; Dalichaouch, Y.; Kohara, T.; Rossel, C.; Torikachvili, M.S.; McElfresh, M.W.; Thompson, J.D.

    1986-01-01

    Transport, thermal, and magnetic data for the heavy electron system URu 2 Si 2 indicate that a charge- or spin-density-wave transition opens an energy gap of approx.11 meV over a portion of the Fermi surface below T 0 roughly-equal17.5 K and demonstrate that bulk superconductivity occurs below T/sub c/roughly-equal1.5 K. The pressure dependences of T 0 and T/sub c/ support this interpretation. The unusually large initial slope of the upper critical magnetic field (9.2 T/K) is consistent with the high values of the electronic-specific-heat coefficient and the electrical resistivity

  13. Unusual temperature dependence of the magnetic moment in URu2Si2

    International Nuclear Information System (INIS)

    Faak, B.; Flouquet, J.; Lejay, P.

    1994-01-01

    The influence of the sample quality on the magnetic properties of the heavy-fermion superconductor URu 2 Si 2 has been studied by elastic neutron scattering. Two single crystals prepared under identical conditions received different heat treatments. The as-grown crystal shows an unusual temperature dependence of the magnetic Bragg peak intensity. The annealed sample behaves normally. The low-temperature magnetic moment is identical for the two samples, showing that the small moment of 0.023 (3) μ B is intrinsic. By varying the instrumental resolution, we show that the ordered moment as well as the limited correlation length (200-400 A) are of static origin. The finite correlation length appears related to defects. (author). 9 refs., 1 fig

  14. Quadrupolar order, hidden octupolar order and tiny magnetic moment in URu2Si2

    International Nuclear Information System (INIS)

    Tsuruta, Atsushi; Matsuura, Tamifusa; Kuroda, Yoshihiro

    2000-01-01

    Possible orders in URu 2 Si 2 are investigated using a two-channel degenerate Anderson model. The ground state of uranium ions is the non-Kramers quadrupolar doublet Γ 5 with (5f) 2 , and its relevant excited state is the Kramers dipolar doublet Γ 7 with (5f) 1 . These states mix with each other via conduction electrons. At low temperatures, the system forms renormalized bands with both quadrupole and dipole degrees of freedom due to the quadrupolar Kondo effect which slightly mixes quadrupolar Γ 5 , a primary state of uranium ions, with dipolar Γ 7 . At a certain low temperature, conduction electrons in the renormalized bands undergo quadrupolar ordering with a large quadrupolar moment. At a further lower temperature, octupolar ordering occurs, accompanied by a tiny dipolar moment which is attributed to the property of the renormalized bands with primarily the Γ 5 -character slightly mixed with the Γ 7 -character. These phenomena are well described by the 1/N-expansion method with pseudo-fermions for the non-Kramers doublet Γ 5 and slave bosons for the Kramers doublet Γ 7 . (author)

  15. Magnetic properties of URu2Si2 under uniaxial stress by neutron scattering

    International Nuclear Information System (INIS)

    Bourdarot, Frederic; Martin, Nicolas; Raymond, Stephane; Regnault, Louis-Pierre; Aoki, Dai; Taufour, Valentin; Flouquet, Jacques

    2011-01-01

    The aim of this study is to compare the magnetic behavior of URu 2 Si 2 under uniaxial stress along the a axis with the behavior under hydrostatic pressure. Both are very similar, but uniaxial stress presents a critical stress σ x a [0.33(5) GPa] that is smaller than the hydrostatic critical pressure p x (0.5 GPa) where the ground state switches from a HO (hidden-order) to AF (antiferromagnetic) ground state. From these critical values and Larmor neutron diffraction, we conclude that the magnetic properties are governed by the shortest U-U distance in the plane (a lattice parameter). Under stress, the orthorhombic unit cell stays centered. A key point shown by this study is the presence of a threshold for the uniaxial stress along the a axis before the appearance of the large AF moment, which indicates no mixture of the order parameter between the HO ground state and the AF one as under hydrostatic pressure. The two most intense longitudinal magnetic excitations at Q 0 =(1,0,0) and Q 1 =(0.6,0,0) were measured in the HO state: the excitation at Q 0 decreases in energy while the excitation at Q 1 increases in energy with the uniaxial stress along the a axis. The decrease of the energy of the excitation at Q 0 seems to indicate a critical energy-gap value of 1.2(1) meV at σ x a . A similar value was derived from studies under hydrostatic pressure at p x .

  16. Tuning of Hidden Order and Superconductivity in URu2Si2 by Applied Pressure and Re Substitution

    International Nuclear Information System (INIS)

    Nicholas P. Butch; Jason R. Jeffries; Benjamin T. Yukich; M. Brian Maple

    2006-01-01

    Single crystals of URu2-xRexSi2 have been grown via the Czochralski technique. Detailed electrical transport studies under pressure on single crystals of URu2Si2 confirm that the zero- temperature critical field is suppressed smoothly towards an extrapolated critical pressure of 15 kbar, which also corresponds to the accepted critical pressure of the hidden order phase. Improving on previous work on polycrystalline samples, studies of single crystals of URu2-xRexSi2 have provided more precise tracking of the suppression of both the hidden order phase at low doping and the ferromagnetic phase at intermediate Re concentrations

  17. Momentum-resolved hidden-order gap reveals symmetry breaking and origin of entropy loss in URu2Si2

    Science.gov (United States)

    Bareille, C.; Boariu, F. L.; Schwab, H.; Lejay, P.; Reinert, F.; Santander-Syro, A. F.

    2014-07-01

    Spontaneous symmetry breaking in physical systems leads to salient phenomena at all scales, from the Higgs mechanism and the emergence of the mass of the elementary particles, to superconductivity and magnetism in solids. The hidden-order state arising below 17.5 K in URu2Si2 is a puzzling example of one of such phase transitions: its associated broken symmetry and gap structure have remained longstanding riddles. Here we directly image how, across the hidden-order transition, the electronic structure of URu2Si2 abruptly reconstructs. We observe an energy gap of 7 meV opening over 70% of a large diamond-like heavy-fermion Fermi surface, resulting in the formation of four small Fermi petals, and a change in the electronic periodicity from body-centred tetragonal to simple tetragonal. Our results explain the large entropy loss in the hidden-order phase, and the similarity between this phase and the high-pressure antiferromagnetic phase found in quantum-oscillation experiments.

  18. Reply to ''Comment on 'Shape of the upper-critical-field curves in URu2Si2: Evidence for anisotropic pairing' ''

    International Nuclear Information System (INIS)

    Joynt, R.; Kwok, W.K.; Crabtree, G.W.; Hinks, D.G.; DeLong, L.

    1991-01-01

    We present an alternate interpretation to the comments by P. Thalmeier [preceding paper, Phys. Rev. B 44, 7120 (1991)] based on the assumption that the antiferromagnetic transition is a secondary effect of some other phase transition at T N [C. M. Varma (unpublished); see also Palstra et al., Phys. Rev. Lett. 55, 2727 (1985)]. This view is motivated by the observation that the ordered moment in URu 2 Si 2 is very small (∼0.02μ B ) and similar to the ordered moment in UPt 3 , another heavy-fermion system, and yet the specific-heat anomaly is at least 2 orders of magnitude larger in URu 2 Si 2 than in UPt 3

  19. Interplay between magnetic quantum criticality, Fermi surface and unconventional superconductivity in UCoGe, URhGe and URu2Si2

    International Nuclear Information System (INIS)

    Bastien, Gael

    2017-01-01

    This thesis is concentrated on the ferromagnetic superconductors UCoGe and URhGe and on the hidden order state in URu 2 Si 2 . In the first part the pressure temperature phase diagram of UCoGe was studied up to 10.5 GPa. Ferromagnetism vanishes at the critical pressure pc≅1 GPa. Unconventional superconductivity and non Fermi liquid behavior can be observed in a broad pressure range around pc. The superconducting upper critical field properties were explained by the suppression of the magnetic fluctuations under field. In the second part the Fermi surfaces of UCoGe and URhGe were investigated by quantum oscillations. In UCoGe four Fermi surface pockets were observed. Under magnetic field successive Lifshitz transitions of the Fermi surface have been detected. The observed Fermi surface pockets in UCoGe evolve smoothly with pressure up to 2.5 GPa and do not show any Fermi surface reconstruction at the critical pressure pc. In URhGe, three heavy Fermi surface pockets were detected by quantum oscillations. In the last part the quantum oscillation study in the hidden order state of URu 2 Si 2 shows a strong g factor anisotropy for two Fermi surface pockets, which is compared to the macroscopic g factor anisotropy extracted from the upper critical field study. (author) [fr

  20. Recent advances in the 5f-relevant electronic states and unconventional superconductivity of actinide compounds

    International Nuclear Information System (INIS)

    Haga, Yoshinori; Sakai, Hironori; Kambe, Shinsaku

    2007-01-01

    Recent advances in the understanding of the 5f-relevant electronic states and unconventional superconducting properties are reviewed in actinide compounds of UPd 2 Al 3 . UPt 3 , URu 2 Si 2 , UGe 2 , and PuRhGa 5 . These are based on the experimental results carried out on high-quality single crystal samples, including transuranium compounds, which were grown by using combined techniques. The paring state and the gap structure of these superconductors are discussed, especially for the corresponding Fermi surfaces which were clarified by the de Haas-van Alphen experiment and the energy band calculations. A detailed systematic study using the NQR/NMR spectroscopy reveals the d-wave superconductivity in PuRhGa 5 and the difference of magnetic excitations due to the difference of ground states in U-, Np-, and Pu-based AnTGa 5 (T: transition metal) compounds. (author)

  1. Study of magnetic structure of neptunium compounds: Np As, Np Sb, Np Se et Np Ru2 Si2

    International Nuclear Information System (INIS)

    Bonnisseau, D.

    1987-11-01

    Magnetic behavior and localization of 5f electrons in actinide compounds is studied experimentally by Moessbauer spectroscopy and neutron diffraction. Binary actinide compounds with a NaCl structure are examined and properties of U, Pu and Np monopnictides and monochalcogenides are recalled. Results of neutron diffraction by NpAs and NpSb are discussed and results of magnetic susceptibility, magnetization, Moessbauer spectroscopy and neutron diffraction measurements on NpSe and NpTe are presented. Magnetic properties of NpRu 2 Si 2 are also presented. Heavy fermion system electronic and magnetic properties are described and theory is discussed. Electronic and magnetic properties of CeCu 2 Si 2 , CeRu 2 Si 2 and URu 2 Si 2 are compared to NpRu 2 Si 2 which has the same crystal structure [fr

  2. Crystal growth of uranium compounds and study of UGe2

    International Nuclear Information System (INIS)

    Taufour, V.

    2011-01-01

    In this thesis, the study on the superconducting ferromagnet UGe 2 is presented. Crystal growth of UGe 2 single crystals was realized in a tetra-arc furnace using the Czochralski technique. This technique was also used to obtain high quality single crystals of other uranium compounds, notably UCoGe and URu 2 Si 2 . The Curie temperature of UGe 2 (T(Curie) = 53 K) decreases with pressure and is suppressed at p c = 1.5 GPa. Before being suppressed, the ferromagnetic transition changes from second to first order at a tricritical point. Precise resistivity and Hall resistivity measurements under pressure and magnetic field revealed the position of the tricritical point as well as its evolution under magnetic field which draw a wing structure phase diagram. Despite the theoretical prediction that this diagram is general for a ferromagnet, here we present the first experimental observation. Other measurements focus on the superconductivity (T sc = 0.75 K) which coexists with ferromagnetism under pressure. The bulk nature of the superconductivity is investigated by AC calorimetry measurements under pressure. The attention is turned to the interesting phenomenon of field enhanced superconductivity. (author) [fr

  3. The degree of 5f electron localization in URu2Si2: electron energy-loss spectroscopy and spin-orbit sum rule analysis

    Energy Technology Data Exchange (ETDEWEB)

    Jeffries, J R; Moore, K T; Butch, N P; Maple, M B

    2010-05-19

    We examine the degree of 5f electron localization in URu{sub 2}Si{sub 2} using spin-orbit sum rule analysis of the U N{sub 4,5} (4d {yields} 5f) edge. When compared to {alpha}-U metal, US, USe, and UTe, which have increasing localization of the 5f states, we find that the 5f states of URu{sub 2}Si{sub 2} are more localized, although not entirely. Spin-orbit analysis shows that intermediate coupling is the correct angular momentum coupling mechanism for URu{sub 2}Si{sub 2} when the 5f electron count is between 2.6 and 2.8. These results have direct ramifications for theoretical assessment of the hidden order state of URu{sub 2}Si{sub 2}, where the degree of localization of the 5f electrons and their contribution to the Fermi surface are critical.

  4. Structural determination of organic compounds

    International Nuclear Information System (INIS)

    Kintzinger, J.P.

    1991-01-01

    This paper reports that the current methods available in high-field NMR spectroscopy are such that the tridimensional structure determination of any rigid molecule containing only carbon and hydrogen atoms may be achieved. The connectivities between carbon-carbon, carbon-hydrogen, and hydrogen-hydrogen atoms are determined by multipulse and two-dimensional (2D) experiments. These connectivity patterns or maps allow a step-by-step reconstruction of the molecular structures. From the carbon-carbon connectivity map, the carbon framework of the molecule is obtained, whereas the carbon-hydrogen pattern allows determination of the positions of the hydrogen atoms on their corresponding carbon atoms. High-field spectrometers are then necessary to remove fortuitous degeneracy and to reduce the proton spectra to a nearly first-order one, allowing an easy measurement of the chemical shifts and the coupling constants

  5. Voltammetric determination of zirconium using azo compounds

    International Nuclear Information System (INIS)

    Orshulyak, O.O.; Levitskaya, G.D.

    2008-01-01

    The optimum conditions for zirconium complexation with azo compounds are found. The applicability of Eriochrome Red B, Calcon, and Calcion to the voltammetric determination of zirconium, total Zr(IV) and Hf(IV), and Zr(IV) in the presence of Zn(II), Cu(II), Cd(II), Ni(II), or Ti(IV) is demonstrated. The developed procedures are used to determine zirconium in a terbium alloy and in an alloy for airplane wheel drums [ru

  6. Carbon determination in uranium and its compounds

    International Nuclear Information System (INIS)

    Silva Queiroz, C.A. da; Abrao, A.

    1982-01-01

    Carbon content in uranium and its compounds, especially ceramic grade UO 2 , must be controlled rigorously. A method for the determination of carbon with the aid of commercial equipment which uses platinum as a catalyst for the oxidation of CO, and infrared cells for CO 2 measurement is described. The detection limit is 5μg C/g U and the determination range is 0.0005 to 5% C/U. The method is being used routinely to control the carbon content in nuclear fuel materials. (Author) [pt

  7. Determination of Phenolic Compounds in Wines

    Directory of Open Access Journals (Sweden)

    Charalampos Proestos

    2012-04-01

    Full Text Available Normal 0 false false false MicrosoftInternetExplorer4 Wine contains natural antioxidants such as phenolic compounds also known as bioactive compounds. Samples of commercially available Greek wines were analyzed in order to determine this phenolic content. For the analysis, Reversed Phase-High Performance Liquid Chromatography (RP-HPLC coupled with a multiwavelength Ultraviolet/visible (UV/vis detector was used. The most abundant phenolic substances detected were (+-catechin (13.5-72.4 mg L-1 , gallic acid (0.40-99.47 mg L-1 and caffeic acid (0.87-33.48 mg L-1. The principal component analysis (PCA technique was used to study differentiation among wines according to their production area. Red wines contained more phenolic substances than white ones. Differences of the phenolic composition in wines of the same cultivar were investigated too.

  8. Spin excitations and the electronic specific heat of URu2Si2

    DEFF Research Database (Denmark)

    Mason, T.E.; Buyers, W.J.L.

    1991-01-01

    We have calculated the mass enhancement due to the interaction of conduction electrons with spin fluctuations, using the generalized spin susceptibility determined from neutron-scattering measurements, for the heavy-fermion superconductor URu2Si2. Reasonable coupling between the spin excitations ...

  9. Determination of arsenic compounds in earthworms

    Energy Technology Data Exchange (ETDEWEB)

    Geiszinger, A.; Goessler, W.; Kuehnelt, D.; Kosmus, W. [Karl-Franzens-Univ., Graz (Austria). Inst. for Analytical Chemistry; Francesconi, K. [Odense Univ. (Denmark). Inst. of Biology

    1998-08-01

    Earthworms and soil collected from six sites in Styria, Austria, were investigated for total arsenic concentrations by ICP-MS and for arsenic compounds by HPLC-ICP-MS. Total arsenic concentrations ranged from 3.2 to 17.9 mg/kg dry weight in the worms and from 5.0 to 79.7 mg/kg dry weight in the soil samples. There was no strict correlation between the total arsenic concentrations in the worms and soil. Arsenic compounds were extracted from soil and a freeze-dried earthworm sample with a methanol/water mixture (9:1, v/v). The extracts were evaporated to dryness, redissolved in water, and chromatographed on an anion- and a cation-exchange column. Arsenic compounds were identified by comparison of the retention times with known standards. Only traces of arsenic acid could be extracted from the soil with the methanol/water (9:1, v/v) mixture. The major arsenic compounds detected in the extracts of the earthworms were arsenous acid and arsenic acid. Arsenobetaine was present as a minor constituent, and traces of dimethylarsinic acid were also detected. Two dimethylarsinoyltribosides were also identified in the extracts by co-chromatography with standard compounds. This is the first report of the presence of dimethylarsinoylribosides in a terrestrial organism. Two other minor arsenic species were present in the extract, but their retention times did not match with the retention times of the available standards.

  10. Determination of Phytochemical Compounds, and Tyrosinase ...

    African Journals Online (AJOL)

    Purpose: To determine the phytochemical content, and tyrosinase inhibitory and antimicrobial activities of the wood ... problems from current whitening cosmetics such as ochronosis ... antibiotics may lead to drug resistance of many bacterial ...

  11. Simultaneous determination of ten compounds in two main ...

    African Journals Online (AJOL)

    Simultaneous determination of ten compounds in two main medicinal plant parts of Tibetan herb, Pterocephalus hookeri (CB Clarke) Höeck, by ultra-high performance liquid chromatography-photodiode array.

  12. Determination of hydrogen isotope composition in organic compounds

    International Nuclear Information System (INIS)

    Ordzhonikidze, K.G.; Parulava, L.P.; Vakhaniya, G.V.; Tarielashvili, V.O.

    1989-01-01

    method for determination of hydrogen isotope composition just in organic compounds using mass-spectrometer of the second class is suggested. The method enables to determine atomic fraction of hydrogen without multiplet separation. The accuracy of determination of deuterium atomic fraction in acetone in 1-99% range was equal to 3-0.2% respectively

  13. Gas chromatographic determination of impurities of inorganic compounds

    International Nuclear Information System (INIS)

    Drugov, Yu.S.

    1985-01-01

    Methods of concentration, separation, detection in gas chromatographic determination of impurities of inorganic compounds including low-boiling gases, reactive gases, organometallic compounds, free metals, anions, etc. are reviewed. Methods of reaction gas chromatography for determining reactive gases, water, anions, metal chelates are considered in detail as well as methods of reaction-sorption concentration and reaction gas extraction. The application of gas chromatograpny ior anaiysis of water and atmosphere contamination, for determination of impurities in highly pure solid substances and gases is described

  14. Analysis of uranium and its compounds. Ruthenium spectrographic determination

    International Nuclear Information System (INIS)

    Anon.

    Ruthenium determination in uranium and its compounds, suitable for content greater than 0.1 ppm with respect to uranium, by dissolution in sulfuric acid and addition of palladium as an internal standard, separation of the precipitated ruthenium, in the presence of gold, by reduction with zinc, the precipitate is calcined and ruthenium is determined by spectrography [fr

  15. Determination of heats of formation of compounds melting incongruently

    Energy Technology Data Exchange (ETDEWEB)

    Kesler, Y.A.; Cheshnitskii, S.M.; Fotiev, A.A.; Tret' yakov, Y.D.

    1985-09-01

    Of significant interest is the development of new procedures for experimental determination of heats of formation of compounds, making it possible to expand the range of substances for which the standard, well-developed methods are unacceptable. The use of hightemperature Calvet microcalorimeters offers great possibilities for this. They recently have been used to determine the most important thermodynamic characteristics of many inorganic substances. In this paper the authors consider the use of drop calorimetry, i.e., the dropping of a sample thermostated at 298/sup 0/K into a calorimeter cell kept at a preassigned temperature for the study of peritecticdecomposition reactions of compounds, to determine their heats of formation. The authors used the compounds Fe/sub 2/V/sub 4/O/sub 13/ and FeVO/sub 4/, as well as high-purity V/sub 2/O/sub 5/.

  16. Determination of borneol and other chemical compounds of ...

    African Journals Online (AJOL)

    Purpose: To determine borneol and other chemical compounds of essential oil derived from the exudate of Dryobalanops aromatica in Malaysia. Methods: Exudate was collected from D. aromatica and subjected to fractional distillation to obtain essential oil. Gas chromatography-mass spectrometry (GC-MS) was performed ...

  17. Determination of oxygen in uranium compounds using sulfur monochloride

    International Nuclear Information System (INIS)

    Baudin, G.; Besson, J.; Blum, P.L.; Tran-Van, Danh

    1964-01-01

    The authors have described in an other paper (Anal. Chim. Acta, in press) a method for oxygen determination in uranium compounds, in which the sample is attacked by sulfur monochloride. The present paper is concerned with the experimental aspects of the method: apparatus procedure. (authors) [fr

  18. Determination of Volatile Organic Compounds in Selected Strains of Cyanobacteria

    Directory of Open Access Journals (Sweden)

    Ivan Milovanović

    2015-01-01

    Full Text Available Microalgal biomass can be used in creating various functional food and feed products, but certain species of microalgae and cyanobacteria are known to produce various compounds causing off-flavour. In this work, we investigated selected cyanobacterial strains of Spirulina, Anabaena, and Nostoc genera originating from Serbia, with the aim of determining the chemical profile of volatile organic compounds produced by these organisms. Additionally, the influence of nitrogen level during growth on the production of volatile compounds was investigated for Nostoc and Anabaena strains. In addition, multivariate techniques, namely, principal component analysis (PCA and hierarchical cluster analysis (HCA, were used for making distinction among different microalgal strains. The results show that the main volatile compounds in these species are medium chain length alkanes, but other odorous compounds such as 2-methylisoborneol (0.51–4.48%, 2-pentylfuran (0.72–8.98%, β-cyclocitral (0.00–1.17%, and β-ionone (1.15–2.72% were also detected in the samples. Addition of nitrogen to growth medium was shown to negatively affect the production of 2-methylisoborneol, while geosmin was not detected in any of the analyzed samples, which indicates that the manipulation of growth conditions may be useful in reducing levels of some unwanted odor-causing components.

  19. Determination of formation enthalpies of incongruently fusing compounds

    International Nuclear Information System (INIS)

    Kesler, Ya.A.; Cheshnitskij, S.M.; Fotiev, A.A.; Tret'yakov, Yu.D.

    1985-01-01

    Using the method of drop-calorimetry i.e. drop into the calorimeter cell being at the specified temperature of the specimen thermostated at 298 K, for studying reactions of peritectic decomposition of compounds for determining their formation enthalpies is considered. The measurements have been performed at 973 K using high temperature double microcalorimeter. The values ΔH 1 =(367.0+-2.8) kJ/mol and ΔH 2 =)343.9+-3.1) kJ/mol are obtained as a result of two series of measurements (6 experiments in each). The advantage of the described technique consists in the fact that the value of enthalpy of compound formation is obtained as a result of direct calorimetric measurements while in the e.m.f. method this value is determined as a coefficient in the Gibbs energy temperature dependence. The method is simple and does not require much time (one measurement takes 30-40 min)

  20. Determination of chlorine in nuclear-grade uranium compounds

    International Nuclear Information System (INIS)

    Yang Chunqing; Liu Fuyun; Huang Dianfan

    1988-01-01

    The determination of chlorine in nuclear-grade uranium compounds is discribed. Chlorine is separated from uranium oxide pyrohydrolytically with stream of wet oxygen in a furnace at 800 ∼ 900 deg C. Chlorine is volatilized as hydrochloric acid, absorbed in a dilute alkaline solution and measured with chlorine-selective electrode. This method covers the concentration range of 10 ∼ 500 pm chlorine in uranium oxide. Precision of at least ± 10% and recovery of 85 ∼ 108% have been reported

  1. Structural determination of some uranyl compounds by vibrational spectroscopy

    International Nuclear Information System (INIS)

    Rodriguez S, A.; Martinez Q, E.

    1990-07-01

    The vibrational spectra of different uranyl compounds has been studied and of it spectral information has been used the fundamental asymmetric vibrational frequency, to determine the length and constant bond force U=O by means of the combination of the concept of absorbed energy and the mathematical expression of Badger modified by Jones. It is intended a factor that simplifies the mathematical treatment and the results are compared with the values obtained for other methods. (Author)

  2. Methods of Selenium Supplementation: Bioavailability and Determination of Selenium Compounds.

    Science.gov (United States)

    Bodnar, Malgorzata; Szczyglowska, Marzena; Konieczka, Piotr; Namiesnik, Jacek

    2016-01-01

    Selenium, a "dual-surface" element, maintains a very thin line between a level of necessity and harmfulness. Because of this, a deficiency or excess of this element in an organism is dangerous and causes health-related problems, both physically and mentally. The main source of selenium is a balanced diet, with a proper selection of meat and plant products. Meanwhile, the proper assimilation of selenium into these products depends on their bioavailability, bioaccessibility, and/or bioactivity of a given selenium compound. From the time when it was discovered that selenium and its compounds have a significant influence on metabolic processes and in many countries throughout the world, a low quantity of selenium was found in different parts of the environment, pressure was put upon an effective and fast method of supplementing the environment with the help of selenium. This work describes supplementation methods applied with the use of selenium, as well as new ideas for increasing the level of this element in various organisms. Based on the fact that selenium appears in the environment at trace levels, the determination of total amount of selenium or selenium speciation in a given sample demands the selection of appropriate measurement methods. These methods are most often comprised of a sample preparation technique and/or a separation technique as well as a detection system. The work presents information on the subject of analytical methods used for determining selenium and its compounds as well as examples in literature of their application.

  3. Determination of carbonyl compounds in air by HPLC

    International Nuclear Information System (INIS)

    Garcia, S.; Perez, R.M.; Campos, A.; Gonzalez, D.

    1995-09-01

    A method for the determination of seven carbonyl compounds in air is presented. The procedure involve sampling of air by a Sep-Pak cartridge impregnated with 2,4-dinitrophenylhydrazine. Elution was done with 3 mL of acetonitrile and the eluate was diluted to 5 mL. The analysis was done by HPLC with UV detection and external standard method quantification. It has been achieved relative standard deviations about 5% and detection limits of 80 ng/cartridge for formaldehyde, acetaldehyde and acetone+acrolein. Three different types of samples (rural, urban, petrol emission) were successfully analyzed

  4. Determination of carbonyl compounds in air by HPLC

    International Nuclear Information System (INIS)

    Garcia, S.; Perez, R.M.; Campos, A.; Gonzalez, D.

    1995-01-01

    A method for the determination of seven carbonyl compounds in air is presented. The procedure involve sampling of air by a Sep-Pak Cartridge impregnated with 2,4-dinitrophenylhydrazine. Elution was done with 3 mL of acetonitrile and the eluate was diluted to 5 mL. The analysis was done by HPLC with UV detection and external standard method quantification. It has been achieved relative standard deviations about 5% and detection limits of 80 ng/cartridge for formaldehyde, acetaldehyde and acetoacetonitrile. Three different types of samples (rural, urban, petrol emission) were successfully analyzed. (Author) 12 refs

  5. Determination of organic compounds in water using ultraviolet LED

    Science.gov (United States)

    Kim, Chihoon; Ji, Taeksoo; Eom, Joo Beom

    2018-04-01

    This paper describes a method of detecting organic compounds in water using an ultraviolet LED (280 nm) spectroscopy system and a photodetector. The LED spectroscopy system showed a high correlation between the concentration of the prepared potassium hydrogen phthalate and that calculated by multiple linear regression, indicating an adjusted coefficient of determination ranging from 0.953-0.993. In addition, a comparison between the performance of the spectroscopy system and the total organic carbon analyzer indicated that the difference in concentration was small. Based on the close correlation between the spectroscopy and photodetector absorbance values, organic measurement with a photodetector could be configured for monitoring.

  6. Determination of formation enthalpies of incongruently fusing compounds

    Energy Technology Data Exchange (ETDEWEB)

    Kesler, Ya.A.; Cheshnitskij, S.M.; Fotiev, A.A.; Tret' yakov, Yu.D.

    1985-04-01

    Using the method of drop-calorimetry i.e. drop into the calorimeter cell being at the specified temperature of the specimen thermostated at 298 K, for studying reactions of peritectic decomposition of compounds for determining their formation enthalpies is considered. The measurements have been performed at 973 K using high temperature double microcalorimeter. The values ..delta..H/sub 1/=(367.0 +- 2.8) kJ/mol and ..delta..H/sub 2/=)343.9 +- 3.1) kJ/mol are obtained as a result of two series of measurements (6 experiments in each). The advantage of the described technique consists in the fact that the value of enthalpy of compound formation is obtained as a result of direct calorimetric measurements while in the e.m.f. method this value is determined as a coefficient in the Gibbs energy temperature dependence. The method is simple and does not require much time (one measurement takes 30-40 min).

  7. [Compound preservative and cyclamat determinated by gas chromatography].

    Science.gov (United States)

    Xin, Ruozhu; Ding, Mei; Zheng, Xianguang; Li, Yajuan

    2008-07-01

    To establish a gas chromatography method for synchronous determination of six preservatives and cyclamat in cake and pastry. The pre-treatment of complicated compound was finished by dialysis cleaning technology. The interference of the complicated foundation body in the cake and pastry was removed by the best dialysis condition: 2 g/L NaOH of dialysis fluid was dialyzed at the temperature of 25 degrees C for 24h, and the six preservatives and cyclamat (sorbic acid, benzoic acid, dehydroacetic acid, ethylparabenum, propylparabenum, butylparabenun and sodium cyclamate) were synchronously seperated by 60-80 mesh Chromosorb WAW DMCS glass packing column of intercoated 5% DEGS + 1% H3 PO4. The seven components in the sample had a good lining relation at the concentration 100 -5000 mg/L when the external standard method was used, and their correlation coefficients were 0.9993-0.9998, and their average recovery rates were 87.5%-101.9%, and their relative standard deviations were 0.64%-3.3%, and detection limits were 1.1-8.8 mg/L. This method could be used to quickly analyse the compound preservatives of the large batch cake and pastry through the common gas chromatography and packed column and this method was simple, accurate and quick.

  8. Spectrographic determination of some rare earths in thorium compounds

    International Nuclear Information System (INIS)

    Brito, J. de.

    1977-01-01

    A method for spectrographic determination of Gd, Sm, Dy, Eu, Y, Yb, Tm and Lu in thorium compounds has been developed. Sensibilities of 0.01 μg rare earths/g Th02 were achieved. The rare earth elements were chromatographycally separated in a nitric acid-ether-cellulose system. The solvent mixture was prepared by dissolving 11% of concentrated nitric acid in ether. The method is based upon the sorption of the rare earths on activated cellulose, the elements being eluted together with 0.01 M HNO 3 . The retention of the 152 , 154 Eu used as tracer was 99,4%. The other elements showed recoveries varying from 95 to 99%. A direct carrier destillation procedure for the spectrochemical determination of the mentioned elements was used. Several concentrations of silver chloride were used to study the volatility behavior of the rare earths. 2%AgCl was added to the matrix as definite carrier, being lantanum selected as internal standard. The average coefficient of variation for this method was +- -+ 7%. The method has been appleid to the analysis of rare earths in thorium coumpounds prepared by Thorium Purification Pilot Plant at Atomic Energy Institute, Sao Paulo [pt

  9. Quantitative method of determining beryllium or a compound thereof in a sample

    Science.gov (United States)

    McCleskey, T. Mark; Ehler, Deborah S.; John, Kevin D.; Burrell, Anthony K.; Collis, Gavin E.; Minogue, Edel M.; Warner, Benjamin P.

    2010-08-24

    A method of determining beryllium or a beryllium compound thereof in a sample, includes providing a sample suspected of comprising beryllium or a compound thereof, extracting beryllium or a compound thereof from the sample by dissolving in a solution, adding a fluorescent indicator to the solution to thereby bind any beryllium or a compound thereof to the fluorescent indicator, and determining the presence or amount of any beryllium or a compound thereof in the sample by measuring fluorescence.

  10. Determination of methylmercury compounds in foodstuffs. II. Determination of methylmercury in fish, egg, meat, and liver

    Energy Technology Data Exchange (ETDEWEB)

    Westoeoe, G

    1967-01-01

    The combined gas chromatographic and thin-layer chromatographic method for the identification and determination of methylmercury compounds in fish (Westoeoe) has been modified in order to render it applicable to a wider range of foods. In animal foodstuffs methylmercury is probably to a great extent attached to thiol groups. When these foods are extracted according to Gage, methylmercury chloride is formed and dissolves in the benzene together with varying amounts of thio compounds. Purification of the methylmercury in the benzene extracts of e.g., egg yolk or liver by extraction with aqueous alkali solution did not work, probably because the thio compounds were not volatile and could form alkali-insoluble methylmercury salts. Evidently methylmercury-S-compounds were reformed at high pH and prevented the formation of the water-soluble methylmercury hydroxide. Addition of excess mercuric ions, which expelled the methylmercury from the thio compounds, solved this clean-up problem. Samples of fish, egg-white, egg yolk, meat, and liver have been analyzed with the modified method. Extraction of the methylmercury into an aqueous phase was also possible with the aid of a water solution of cysteine. This led to a more rapid analytical procedure. 8 references, 2 figures, 4 tables.

  11. Determination of Volatile Compounds of Illicium verum Hook. f ...

    African Journals Online (AJOL)

    02.1 mass spectral library in MSD ChemStation. Relative content of each compound in essential oil was calculated by peak area normalization method. These compounds accounted for more than 90 % in total star anise aroma molecules, including trans-anethole (75.76 %), p- anisaldehyde (8.65 %), estragole (4.70 %),.

  12. Determination of an Effective Perfluorinated Compounds (PFCs) Oxidation Method

    Science.gov (United States)

    Siriwardena, D. P.; Crimi, M.; Holsen, T.; Bellona, C.

    2014-12-01

    Perfluoroalkyl and polyfluoroalkyl substances (PFASs) are a stable synthetic class of chemicals ubiquitously spread in environmental media (i.e. air, soil, biota, surface water and groundwater). The substances' strong polar carbon-fluorine bonds and their high thermal and chemical stability make them resistant to biological, chemical, and physical degradation. The purpose of this research is to identify the most effective oxidation method to treat perfluorinated compounds (PFCs) and their by-products that is suitable for in situ application. The laboratory oxidation study focuses on the more commonly detected and studied long-chain (C-8) PFAS; perfluorooctanoic acids (PFOA) and perfluorooctane sulfonic acid (PFOS). Existing research evaluating oxidizing treatment effectiveness on perfluoroalkyl sulfoinoic acids (PFSAs) is limited. A review of the literature and results from preliminary studies indicate that activated persulfate and catalyzed hydrogen peroxide propagation (CHP) reactions appear to be promising oxidants for PFOA. It has been demonstrated that the reactivity of superoxide in water increases in the presence of hydrogen peroxide (H2O2) and solids. Superoxide generated in CHP reactions degrades PFOA seemingly similar to superoxide-mediated destruction of the perhalogenated compounds.The goal of this study is to look at conditions that promote generation of superoxide and look at PFASs treatment effectiveness and byproduct generation. CHP reactions are conducted with varying amount of H2O2 and Fe(III) to determine the optimum conditions for PFC degradation. Results will be compared to those of another experiment using manganese dioxide as a CHP catalyst with varied H2O2 concentration to generate superoxide to degrade PFASs. Activated persulfate conditions to be compared include alkaline pH activation, heat activation, and dual oxidation (combined H2O2 and persulfate ). This presentation will focus on a comparison of oxidation effectiveness under the

  13. Simultaneous determination of ten compounds in two main ...

    African Journals Online (AJOL)

    attempts were made to distinguish different medicinal parts of P. hookeri. Results: Regression equation for 10 compounds showed good linear regression (R2 > 0.9994). The relative standard deviations of precision, stability, repeatability and recovery were under 5 %. Compared with the aerial plant part, the root had ...

  14. Determination of ferulic acid and related compounds by thin layer ...

    African Journals Online (AJOL)

    The analysis of certain phenolic compounds from plants, and their chemical transformation with microorganisms or isolated enzymes, has application in the food and pharmaceutical industry. The rapid quantitative estimation of ferulic acid by thin layer chromatography is described by measurement of the area of the ...

  15. Determination of volatile aroma compounds of Ganoderma lucidum ...

    African Journals Online (AJOL)

    This study was conducted at Horticulture Department of Cukurova University, Adana, Turkey during 2010-2011. Fresh sample of Ganoderma lucidum collected from Mersin province of Turkey was used as material. Volatile aroma compounds were performed by Headspace Gas Chromatography (HS-GC/MS). Alcohols ...

  16. Determination of borneol and other chemical compounds of ...

    African Journals Online (AJOL)

    1Department of Pre-Clinical Sciences, Faculty of Medicine and Health Sciences, Universiti Tunku Abdul Rahman, Lot PT. 21144, Jalan Sungai Long, .... due to geographical variation of plant species, which lead to difference in environmental and culture conditions. In summary, the compounds detected in this study such as ...

  17. New Compounds from Euphorbia helioscopia and Absolute Configuration Determination by Computational Methods

    International Nuclear Information System (INIS)

    He, Jiangbo; Zhu, Hua Jie; Luo, Gui Fen; Li, Yan; Cheng, Yong Xian; Chen, Hao; Chen, Shaopeng; Lu, Xin; Zhou, Guochun; Liu, Guang Ming

    2010-01-01

    The whole plant of Euphorbia helioscopia is an important traditional Chinese medicine. Fom its BuOH soluble extract, one new lactam, three new terpenoids including a new naturally occurring compound, and three known compounds were isolated. Their structures were identified by spectroscopic evidences. In particular, the absolute configurations of side chain of compounds 1 and 2 were determined using computational methods

  18. Determination of gaseous compounds using online mass spectrometry

    International Nuclear Information System (INIS)

    Praun, S.

    1999-08-01

    The work is divided in three major parts and describes various measurements of gaseous compounds. The first part tasks the problem of transit traffic along the motorway from Kufstein, Northern Tyrol/Austria until Ala, Trentino/Italy. During three periods measurements of the immissions of many compounds were carried out simultaneously in Northern Tyrol, Southern Tyrol and Trentino. The influence of the ban of heavy lorry traffic during the weekend and during the night on the reduction of NO 2 could be demonstrated. Furthermore certain compounds (e.g. Benzene) were monitored online for the first time along the motorway at lowest concentrations using the mass spectrometer 'Airsense 500'. In the second part online measurements of exhaled human breath after the oral application of a medicine against bronchitis was performed. In that way beside clinical and pharmacological studies the effectiveness of this pharmacon could be proved. The last part of the present work shows adsorption- and desorption measurements on four different adsorbents. During this procedure seven different gases with an increasing number of carbon atoms were monitored online by the hyphenation of these adsorbents with the mass spectrometer 'Airsense 500'. Thereby, the various properties of the adsorbents in the interaction with the gases could be demonstrated. (author)

  19. Determination of high molecular mass compounds from Amazonian plant's leaves

    International Nuclear Information System (INIS)

    Siqueira, Denilson Soares de; Pereira, Alberto dos Santos; Aquino Neto, Francisco Radler de; Simoneit, Bernd R.T.

    2003-01-01

    The fractions of dichloromethane extracts of leaves from andiroba (Carapa guianensis - Meliaceae), caapi (Banisteriopsis caapi - Malpighiaceae), cocoa (Theobroma cacao - Sterculiaceae), Brazil nut (Bertholletia excelsa - Lecytidaceae), cupuacu (Theobroma grandiflorum - Sterculiaceae), marupa (Simaruba amara - Simaroubaceae) and rubber tree (Hevea brasiliensis - Euphorbiaceae), were analyzed by HT-HRGC and HT-HRGC-MS. Esters of homologous series of fatty acids and long chain alcohols, phytol, amyrines and tocopherols were characterized. The characterization of the compounds was based mainly in mass spectra data and in addition by usual spectrometric data ( 1 H and 13 C NMR, IR). (author)

  20. Determination of Carbonyl Compounds in Exhaled Cigarette Smoke

    Directory of Open Access Journals (Sweden)

    Moldoveanu S

    2014-12-01

    Full Text Available This paper presents the findings on a quantitative evaluation of carbonyl levels in exhaled cigarette smoke from human subjects. The cigarettes evaluated include products with 5.0 mg ‘tar’, 10.6 mg ‘tar’ and 16.2 mg ‘tar’, where ‘tar’ is defined as the weight of total wet particulate matter (TPM minus the weight of nicotine and water, and the cigarettes are smoked following U.S. Federal Trade Commission (FTC recommendations. The measured levels of carbonyls in the exhaled smoke were compared with calculated yields of carbonyls in the inhaled smoke and a retention efficiency was obtained. The number of human subjects included a total of ten smokers for the 10.6 mg ‘tar’, five for the 16.2 mg ‘tar’, and five for the 5.0 mg ‘tar’ product, each subject smoking three cigarettes. The analyzed carbonyl compounds included several aldehydes (formaldehyde, acetaldehyde, acrolein, propionaldehyde, crotonaldehyde and n-butyraldehyde, and two ketones (acetone and 2-butanone. The smoke collection from the human subjects was vacuum assisted. Exhaled smoke was collected on Cambridge pads pretreated with a solution of dinitrophenylhydrazine (DNPH followed by high performance liquid chromatography (HPLC analysis of the dinitrophenylhydrazones of the carbonyl compounds. The cigarette butts from the smokers were collected and analyzed for nicotine. The nicotine levels for the cigarette butts from the smokers were used to calculate the level of carbonyls in the inhaled smoke, based on calibration curves. These were generated separately by analyzing the carbonyls in smoke and the nicotine in the cigarette butts obtained by machine smoking under different puffing regimes. The comparison of the level of carbonyl compounds in exhaled smoke with that from the inhaled smoke showed high retention of all the carbonyls. The retention of aldehydes was above 95% for all three different ‘tar’ levels cigarettes. The ketones were retained with a

  1. Determination of total gas in lithium tritide-deuteride compounds

    International Nuclear Information System (INIS)

    Smith, M.E.; Koski, N.L.; Waterbury, G.R.

    1979-04-01

    Lithium tritide--deuteride samples are enclosed in a copper foil and decomposed by heating to 850 0 C in a copper reaction tube in vacuum. The temperature and pressure of the evolved gas, collected in a measured volume using a Toepler pump, are measured to determine the total moles of gas released from the sample. The gas is transferred to a removable sample bulb and, if required, analyzed for gaseous constituents by mass spectrometry. Based on 14 total gas determinations for a lithium deuteride sample, the calculated relative standard deviation was 1.0% and the estimated bias was <2.5%

  2. Determination of carbon in uranium and its compounds

    International Nuclear Information System (INIS)

    Perez-Garcia, M. M.

    1972-01-01

    This paper collects the analytical methods used our laboratories for the determination of carbon in uranium metal, uranate salts and the oxides, fluorides and carbides of uranium. The carbon is usually burned off in a induction or resistance oven under oxygen flow. The CO 2 is collected in barite solution. Where it is backtitrated with potassium biphthalate. (Author)

  3. Simultaneous determination of oxygen and cadmium in cadmium and cadmium compounds

    International Nuclear Information System (INIS)

    Imaeda, K.; Kuriki, T.; Ohsawa, K.; Ishii, Y.

    1977-01-01

    Cadmium and its compounds were analysed for oxygen and cadmium by a modification of the Schutze-Unterzaucher method. Oxygen in some compounds such as cadmium oxide, nitrate and sulphate could not be determined by the usual method. The method of adding carbon was employed for the determination of total oxygen. Total oxygen could be determined by the addition of 5 mg of carbon to a sample boat and heating at 950 0 . The determination was also carried out by addition of naphthalene (2 mg). It was found that the cadmium powder and cadmium flake used contained ca. 1 and 0.15% oxygen, respectively. Oxygen and cadmium in cadmium and its compounds were simultaneously determined by the addition of 2 mg of naphthalene. Cadmium was determined colorimetrically by use of glyoxal-bis-(2-hydroxyanil). Oxygen and cadmium in the samples could be determined simultaneously with an average error of -0.02 and -0.22%, respectively. (author)

  4. Phenolic compounds and related enzymes as determinants of sorghum for food use

    NARCIS (Netherlands)

    Dicko, M.H.; Gruppen, H.; Traore, A.S.; Voragen, A.G.J.; Berkel, van W.J.H.

    2006-01-01

    Phenolic compounds and related enzymes such as phenol biosynthesizing enzymes (phenylalanine ammonia lyase) and phenol catabolizing enzymes (polyphenol oxidase and peroxidase) are determinants for sorghum utilization as human food because they influence product properties during and after sorghum

  5. Determination of sulfur compounds in hydrotreated transformer base oil by potentiometric titration.

    Science.gov (United States)

    Chao, Qiu; Sheng, Han; Cheng, Xingguo; Ren, Tianhui

    2005-06-01

    A method was developed to analyze the distribution of sulfur compounds in model sulfur compounds by potentiometric titration, and applied to analyze hydrotreated transformer base oil. Model thioethers were oxidized to corresponding sulfoxides by tetrabutylammonium periodate and sodium metaperiodate, respectively, and the sulfoxides were titrated by perchloric acid titrant in acetic anhydride. The contents of aliphatic thioethers and total thioethers were then determined from that of sulfoxides in solution. The method was applied to determine the organic sulfur compounds in hydrotreated transformer base oil.

  6. Application of HPLC-DAD Technique for Determination of Phenolic Compounds in Bee Pollen Loads

    Directory of Open Access Journals (Sweden)

    Waś Ewa

    2017-06-01

    Full Text Available A method was elaborated to determine phenolic compounds (vanillin, caffeic, p-coumaric and salicylic acids, and flavonoids: rutin, hesperetin, quercetin, pinocembrin, apigenin, kaempferol, isorhamnetin, chrysin, and acacetin in bee pollen loads using highperformance liquid chromatography with a diode array detector (HPLC-DAD. Phenolic compounds from bee pollen were isolated on Cleanert C18-SPE columns (500 mg/6 mL, Agela Technologies. Polyphenols were identified by comparing the retention times and spectra of compounds found in pollen load samples with the ones of the standard mixture. Quantitative analysis was conducted using the external standard method. In addition, basic validation parameters for the method were determined. For the identified compounds (except for the salicylic acid, satisfactory (≥0.997 linear correlations were obtained. The elaborated method showed high repeatability and inter-laboratory reproducibility. Variability coeffcients of the majority of phenolic compounds did not exceed 10% in conditions of repeatability and inter-laboratory reproducibility, and for the total polyphenolic content they were 1.7 and 5.1%, respectively. The pollen load samples (n = 15 differed in qualitative and quantitative composition of the phenolic compounds. In all the samples, we identified the p-coumaric and salicylic acids and flavonoids rutin, hesperetin, and apigenin nevertheless, these compounds’ contents significantly differed among individual samples. The total phenolic content in the tested samples of pollen loads ranged from 0.653 to 5.966 mg/100 g (on average 2.737 mg/100 g.

  7. Rapid and accurate determination of radiochemical purity of sup(99m)Tc compounds

    International Nuclear Information System (INIS)

    Tamat, S.R.

    1977-01-01

    The wide spread use of sup(99m)Tc-labelled radiopharmaceuticals and limitation of the short half-life of the isotope, is associated with an urgent need for a rapid, simple but accurate method for determining the radiochemical purity of the compound. A short paper chromatographic (KK) or thin layer chromatographic (KLT) method using 95% methanol or 0.9% saline solution as solvents, has solved the problem. With these methods, the amount of free sup(99m)Tc pertechnetate in a compound, can be determined in only a few minutes. These methods compare satisfactorily with lengtheir procedures. (author)

  8. Determination of volatile compounds of the first rose oil and the first ...

    African Journals Online (AJOL)

    Background: Rose water and rose oil are used in the perfume, cosmetic, pharmaceutical and food industries. The determination of volatile compounds in rose oil and rose water obtained from oil-bearing rose is highly important in terms of availability in the industry and in human health. Materials and Methods: Twenty four ...

  9. Determining order-up-to levels under periodic review for compound binomial (intermittent) demand

    NARCIS (Netherlands)

    Teunter, R. H.; Syntetos, A. A.; Babai, M. Z.

    2010-01-01

    We propose a new method for determining order-up-to levels for intermittent demand items in a periodic review system. Contrary to existing methods, we exploit the intermittent character of demand by modelling lead time demand as a compound binomial process. in an extensive numerical study using

  10. Odour Detection Threshold Determination of Volatile Compounds in Topical Skin Formulations

    DEFF Research Database (Denmark)

    Thomsen, Birgitte Raagaard; Hyldig, Grethe; Taylor, Robert

    2018-01-01

    determination and also odour description by a trained sensory panel. In one case, the odour detection threshold value was 50 times higher (less detectable) in skin care products than in water, whereas for other volatile compounds the odour detection threshold value was only 1.5 times higher. The odour...

  11. The use of voltammetry for determining uranium and associated elements in compounds of nuclear interest

    International Nuclear Information System (INIS)

    Carvalho, F.M.S. de.

    1988-01-01

    The determination of uranium and some trace elements found as impurities in nuclear materials by the voltammetric technique using the hanging mercury drop electrode is presented. Emphasis is given to the determination of uranium, of major interest. Europium and ytterbium are simultaneously determined in fractions of individual lanthanides. A procedure for the simultaneous determination of copper, cadmium, nickel and zinc in water, industrial effluents and uranium compounds is discussed. The advantage of the procedure is its simplicity and easiness of execution, with excellent precision and accuracy. (author) [pt

  12. Influence of organic nitro-compounds and of surface active compounds on the inverse voltametric determination of cadmium, lead and copper

    Energy Technology Data Exchange (ETDEWEB)

    Wahdat, F; Neeb, R

    1983-12-01

    The influence of surface active agents and of organic nitro-compounds alone and in combination on the potentiometric stripping analysis and anodic-stripping differential-pulse-polarography of Cd, Pb and Cu is investigated. In some cases PSA offers advantages for the determination of these elements in the presence of organic nitro-compounds in comparison with differential pulse-polarography.

  13. Separation of halogens from uranium compounds by means of pyrohydrolysis and their determination by ion chromatography

    International Nuclear Information System (INIS)

    Pires, M.A.F.; Brandao Filho, D.; Abrao, A.

    1987-07-01

    This paper describs the determination of fluorine in nuclear grade uranium compounds by means of phyrohydrolysis. A stream of wet oxygem at a temperature of 900 to 1000 0 C is passed through a quartz tube where the powdered samples is put. The halogens are volatilized as their respective acids that are absorbed in a buffer solution or water. The measurements are made with ion-seletive eletrodes or by ion chromatography. The sensitivity is of 1μg F - /g and 5μg Cl - /g. The separation of fluorine from uranium compounds by diferent methods is discussed. (Author) [pt

  14. Separation of chloride and fluoride from uranium compounds and their determination by ion selective electrodes

    International Nuclear Information System (INIS)

    Pires, M.A.F.; Abrao, A.

    1982-01-01

    Fluoride and chloride must be rigorously controlled in uranium compounds, especially in ceramic grade UO 2 . Their determination is very difficult without previous uranium separation, particularly when both are at a low concentration. A simple procedure is described for this separation using a strong cationic resin to retain the uranyl ion. Both anions are determined in the effluent solution. Uranium compounds of nuclear fuel cycle, especially ammonium diuranate, ammonium uranyl tricarbonate, sodium diuranate, uranium trioxide and dioxide and uranium peroxide are dissolved in nitric acid and the solutions are percolated through the resin column. Chloride and fluoride are determined in the effluent by selective electrodes, the detection limits being 0.02 μg F - /ml and 1.0 μg Cl - /ml. The dissolution of the sample, the acidity of the solution, the measurement conditions and the sensitivity of the method are discussed. (Author) [pt

  15. Comparison of SPME Methods for Determining Volatile Compounds in Milk, Cheese, and Whey Powder

    Directory of Open Access Journals (Sweden)

    Michael H. Tunick

    2013-11-01

    Full Text Available Solid phase microextraction and gas chromatography-mass spectrometry (SPME-GC-MS are commonly used for qualitative and quantitative analysis of volatile compounds in various dairy products, but conditions have to be adjusted to maximize release while not generating new compounds that are absent in the original sample. Queso Fresco, a fresh non-melting cheese, may be heated at 60 °C for 30 min; in contrast, compounds are produced in milk when exposed to light and elevated temperatures, so milk samples are heated as little as possible. Products such as dehydrated whey protein are more stable and can be exposed to longer periods (60 min of warming at lower temperature (40 °C without decomposition, allowing for capture and analysis of many minor components. The techniques for determining the volatiles in dairy products by SPME and GC-MS have to be optimized to produce reliable results with minimal modifications and analysis times.

  16. Atomic absorption determination of iron and copper impurities in rare earth compounds

    International Nuclear Information System (INIS)

    Zelyukova, Yu.V.; Kravchenko, J.B.; Kucher, A.A.

    1978-01-01

    An extraction atomic absorption method for the determination of copper and iron impurities in rare earth compounds has been developed. The extraction separation of determined elements as hydroxy quinolinates with isobuthyl alcohol was used. It increased the sensitivity of these element determination and excluded the effect of the analysed sample. Cu, Te, Zn, Bi, Sn, In, Ga, Tl and the some other elements can be determined at pH 2.0-3.0 but rare earths are remained in an aqueous phase. The condition of the flame combustion does not change during the introduction of isobutyl extract but the sensitivity of the determination of the elements increased 2-3 times. The limit of Fe determination is 0.01 mg/ml and the limit of Cu determination is 0.014 mg/ml

  17. Instrumental neutron-activation determination of impurities in lead and titanium compounds

    Energy Technology Data Exchange (ETDEWEB)

    Popova, I L

    1980-01-01

    Instrumental neutron-activation analysis was used to determine 22 impurities in lead and titanium compounds (e.g. PbO, Pb/NO3/2, and TiO2) used as raw materials for ferroelectrics. Five elements (Al, V, Mn, Sc, and Se) were determined by short-lived isotopes and 17 elements were determined by long-lived isotopes. The detection limits were 7 x 10 to the -3rd to 2 x 10 to the -8th %. A substantial difference in concentrations of certain impurity elements has been found in different series of lead and titanium oxides of similar purity.

  18. [Simultaneous determination of ten organotin compounds in polyvinyl chloride plastics using gas chromatography-mass spectrometry].

    Science.gov (United States)

    Li, Ying; Li, Bin; Liu, Li; Zhang, Chen; Wu, Jingwu; Liu, Zhihong; Li, Xintian

    2009-01-01

    A rapid and effective gas chromatography coupled with mass spectrometry method has been developed systematically and studied for the simultaneous determination of 10 organotin compounds, dibutyltin-dichloride (DBT), n-butyltin-trichloride (MBT), triethyltinchloride (TET), fentin-chloride (TPhT), chlorotributylstannane (TBT), tri-n-propyltinchloride (TPrT), diphenyltin-dichloride (DPhT), tetrabutyltin (TeBT), di-n-octyltin-dichloride (DOT), phenyltin trichloride (MPhT)), in polyvinyl chloride (PVC) plastics. The PVC sample was dissolved with tetrahydrofuran and the polymer in the sample was precipitated with methanol, and then the target compounds were derivatized with sodium tetraethylborate and extracted with hexane under ultrasonication. The qualitative and quantitative analysis were carried out by GC-MS and the total ion chromatogram and selected ion chromatogram were obtained. The derivatization and extraction conditions, such as the derivatization time, derivatization pH value, dosages of derivatization reagent and precipitation reagent were optimized. The good linearities, recoveries and precisions were obtained. The linearity ranges were 0.5 - 50 mg/L. The linearity correlation coefficients of 10 organotin compounds were between 0.997 8 and 0.999 7. The average recoveries were 84.23% - 109.1% with relative standard deviations of 4.24% - 10.75%. The established method has been successfully applied to the determination of organotin compounds in PVC plastics.

  19. Microchip electrophoresis with amperometric detection for a novel determination of phenolic compounds in olive oil.

    Science.gov (United States)

    Godoy-Caballero, María del Pilar; Acedo-Valenzuela, María Isabel; Galeano-Díaz, Teresa; Costa-García, Agustín; Fernández-Abedul, María Teresa

    2012-11-07

    The relevance of the development of microchip electrophoresis applications in the field of food analysis is considered in this work. A novel method to determine important phenolic compounds in extra virgin olive oil samples using a miniaturized chemical analysis system is presented in this paper. Three interesting phenolic compounds in olive oil and fruit (tyrosol, hydroxytyrosol and oleuropein glucoside) were studied by end-channel amperometric detection using a 100 μm gold wire as working electrode in glass microchip electrophoresis. The electrochemical behavior of these compounds was studied and the medium to carry out their detection was selected (0.1 M aqueous sulfuric acid). The best conditions for the separation were achieved in sodium tetraborate (10% methanol, pH 9.50) with different concentrations for the sample and the running buffer in order to allow the sample stacking phenomenon. The injection was carried out using 600 V for 3 s and the separation voltage was set at 1000 V. The quality of the method was evaluated through its analytical figures of merit and by its performance on real extra virgin olive oil samples. Determination of these compounds was carried out using the standard addition calibration method with good recoveries.

  20. Method development for the determination of volatile organic compounds in mixed waste

    International Nuclear Information System (INIS)

    Sandoval, W.F.; Rogers, Y.C.; Schappert, M.F.; Boland, K.S.; Spall, W.D.; Wilkerson, C.W. Jr.

    1993-01-01

    While analytical methods exist for the determination of Resource Conservation and Recovery Act (RCRA) listed organic and inorganic compounds in hazardous materials, equivalent methods suitable for the characterization of radioactively contaminated samples are not at the same level of maturity. The Mixed Waste Methods Development Lab. has been established at Los Alamos National Lab. to address the need for such procedures. This presentation will focus on the efforts that have been directed toward the determination of volatile organic compounds (VOCs) in mixed waste matrices. The capabilities of the Mixed Waste Methods Development Lab. will be outlined. Modifications to the containment boxes and analytical instrumentation required for the analyses will be described, as will experimental procedures and system performance benchmarks. Preliminary results from surrogate and real mixed waste matrices will be presented, and future directions for our method development effort will be discussed

  1. Analytical Methodologies for the Determination of Endocrine Disrupting Compounds in Biological and Environmental Samples

    Directory of Open Access Journals (Sweden)

    Zoraida Sosa-Ferrera

    2013-01-01

    Full Text Available Endocrine-disruptor compounds (EDCs can mimic natural hormones and produce adverse effects in the endocrine functions by interacting with estrogen receptors. EDCs include both natural and synthetic chemicals, such as hormones, personal care products, surfactants, and flame retardants, among others. EDCs are characterised by their ubiquitous presence at trace-level concentrations and their wide diversity. Since the discovery of the adverse effects of these pollutants on wildlife and human health, analytical methods have been developed for their qualitative and quantitative determination. In particular, mass-based analytical methods show excellent sensitivity and precision for their quantification. This paper reviews recently published analytical methodologies for the sample preparation and for the determination of these compounds in different environmental and biological matrices by liquid chromatography coupled with mass spectrometry. The various sample preparation techniques are compared and discussed. In addition, recent developments and advances in this field are presented.

  2. Possibilities of analyzing dump and sewage gas, and determination of halogen and sulfur compounds

    Energy Technology Data Exchange (ETDEWEB)

    Eisenmann, R

    1985-01-01

    In connection with the utilization of refuse and sewage gas efficacions analytical methods are gaining increasing importance especially with regard to halogen and sulfur compounds. The paper describes various possibilities to determine those substances. Besides gas chromatography it takes into account classic analytical methods which can be superior in biogas analytics to modern physical processes. The advantages and disadvantages of each method are discussed and practical experiences obtained by their application reported.

  3. Determination of the rates of clearance of insoluble compounds of plutonium from the lung

    International Nuclear Information System (INIS)

    Watts, L.

    1974-04-01

    There are indications that the process of clearance of inhaled insoluble plutonium compounds from the lung may be represented by a model consisting of three exponential phases. A survey of published data on 'in vivo' and bioassay measurements made after 239 PuO 2 inhalation by men and dogs has been carried out, and the half times of the three exponential phases determined as approximately 1 day, 30 days and 500 days. (author)

  4. Classification of wine by determination of bioactive phenolic compounds using high resolution mass spectrometry

    OpenAIRE

    Ivanova, Violeta; Dimovska, Violeta; Mitrev, Sasa; Gulaboski, Rubin; Bogeva, Elena; Petruseva, Dragana; Causon, Tim; Hann, Stephan

    2016-01-01

    In this project proposal, metabolomic fingerprinting of wine samples will be examined using high performance liquid chromatography combined with ion mobility quadruple time-of-flight mass spectrometry (HPLC–IMS-QTOF-MS) for the first time. Bioactive compounds in wines from various red and white varieties produced in Macedonia and Austria from different wine regions and different vintages will be determined for the first time using a non-targeted fingerprinting approach on this analytical plat...

  5. Determination of one-electron reduction potentials of some radiosensitive compounds by pulse radiolysis

    International Nuclear Information System (INIS)

    Zuo Zhihua; Yao Side; Li Hucheng; Lin Nianyun; Jin Yizun

    1994-01-01

    One-electron reduction potential (E 7 1 ) is one of the important parameters of radiosensitive compound with high electron affinity. In this work one-electron reduction potentials of some radiosensitizers, such as Miso, 911, CMNa, SMU-1, SMU-2, SMD, SNN, S 3 and BSO, were determined pulse radiolytically by using anthraquinone-2-sulfate (AQS), duroquinone (DQ) and methyl viologen (MV 2+ ) as references

  6. The Qualitative And Quantitative Determination Of The Phenolic Compounds In Polygonum Convolvulus L. Species, Polygonaceae Family

    Directory of Open Access Journals (Sweden)

    Olaru O T

    2013-06-01

    Full Text Available Introduction: Polygonum convolvulus L. (black bindweed, syn. Fallopia convolvulus (L. Á. Löve, Polygonaceae family is a plant from the spontaneous flora, spread from the plain zone up to the subalpine zone. The objectives of our researches are the qualitative and quantitative determination of polyphenolic compounds from Polygoni convolvuli herba and the choice of the adequate solvent for obtaining an active pharmacological extract.

  7. Ion exchange separation of nitrate from uranium compounds and its determination by spectrophotometry and ion chromatography

    International Nuclear Information System (INIS)

    Pires, M.A.F.; Atalla, L.T.; Abrao, A.

    1985-11-01

    A procedure for the separation of nitrate from uranium compounds by retaintion of uranyl ion on a cationic ion exchanger and its determination in the effluent is described. Nitrate is analysed by the spectrometric method with 1-phenol-2,4-dissulphonic acid. This determination covers the 1 to 10 μg NO - 3 /mL range and requires an amount of 10 to 100 μg NO - 3 . The main interference is uranium (VI) due its own intense yellow color. This difficulty is overcome by the complete separation of UO 2 ++ with the cationic resin. Alternatively, the ion chromatography technique is used for the determination of nitrate in the effluent of the cationic resin. The determination was easily made by the comparison of the nitrate peak hights of the analyte and the standard solutions. The ion chromatography method is very sensitive (0,3 μg NO - 3 /mL), reproducible and suitable for routine analysis and permits the determination of fraction of part per million of nitrate in uranium. The results of nitrate determination using both spectrophotometric and ion chromatography techniques are compared. The method is being routinely applied for the quality control of uranium compounds in the fuel cycle, specially uranium oxide, ammonium diuranate, uranium peroxide and ammonium uranyl tricarbonate. (Author) [pt

  8. Improved Gas Chromatographic Determination of Guanidino Compounds Using Isovaleroylacetone and Ethyl Chloroformate as Derivatizing Reagents.

    Science.gov (United States)

    Zounr, Rizwan Ali; Khuhawar, Mumammad Yar; Jahangir, Taj Muhammad; Alamgir, Malik

    2016-01-01

    An improved GC method in terms of sensitivity and decrease in the analysis time has been developed for the analysis of eight guanidino compounds: guanidine (G), methylguanidine (MG), creatinine (CTN), guanidinoacetic acid (GAA), guanidinobutyric acid (GBA), guanidinopropionic acid (GPA), argenine (Arg), and guanidinosuccinic acid (GSA), using isovaleroylacetone (IVA) and ethyl chloroformate (ECF) as derivatizing reagents. The separation was obtained from column HP-5 (30 m × 0.32 mm i.d.) with film thickness of 0.25 μm within 11 min. The linear calibrations were obtained with 0.5 to 50 μg/mL with coefficient of determination (R(2)) within 0.9969 - 0.9998. Limits of detections (LODs) were within 5 - 140 ng/mL. The derivatization, separation and determination was repeatable (n = 6) with relative standard deviation (RSD) within 1.2 - 3.1%. The guanidino compounds were determined in deproteinized serum of healthy volunteers and uremic patients within below LOD to 8.8 μg/mL and below LOD to 43.99 μg/mL with RSD within 1.4 - 3.6%. The recovery of guanidino compounds calculated by standard addition from serum was within 96.1 - 98.9%, with RSD 1.4 - 3.6%.

  9. Radiochromatographic method for determination of macroenergetic phosphorus compounds in the rat heart muscle

    International Nuclear Information System (INIS)

    Wajdowicz, A.

    1980-01-01

    The 32 P was injected intraperitoneally. After 20 min. a part of heart muscle was taken off under anaesthesia from which phosphorus compounds were extracted and separated by means of paper chromatography. Separation was performed on the Whatman 1 paper, in glass tank produced by Shandon by means of method replacing of two direction descending chromatography use together with three solvent system. Identification of nucleotides was conducted in the UV light, besides CP and inorganic phosphorus by means of chemical methods. For the qualitative analysis of separated phosphorus compounds autoradiography was applied. Quantitative analysis was conducted by means of radiogrametric method. Radioactivity for each of examined phosphorus compounds was computed from chromatograms. Radioactive curves were indicated for each stage of chromatography separation. It was found the peaks on the radioactive curves equal the black spots on the autoradiograms and the spots identified with optical test and by the chemical method. This method permits in constant condition absolute separation and quantitative determination of phosphorus compounds in the rat heart muscle. It is relatively simple and more specific than chemical methods. (author)

  10. Determination of phenolic compounds in air by using cyclodextrin-silica hybrid microporous composite samplers.

    Science.gov (United States)

    Mauri-Aucejo, Adela R; Ponce-Català, Patricia; Belenguer-Sapiña, Carolina; Amorós, Pedro

    2015-03-01

    An analytical method for the determination of phenolic compounds in air samples based on the use of cyclodextrin-silica hybrid microporous composite samplers is proposed. The method allows the determination of phenol, guaiacol, cresol isomers, eugenol, 4-ethylphenol and 4-ethylguaiacol in workplaces according to the Norm UNE-EN 1076:2009 for active sampling. Therefore, the proposed method offers an alternative for the assessment of the occupational exposure to phenol and cresol isomers. The detection limits of the proposed method are lower than those for the NIOSH Method 2546. Storage time of samples almost reaches 44 days. Recovery values for phenol, guaiacol, o-cresol, m-cresol, p-cresol, 4-ethylguaiacol, eugenol and 4-ethylphenol are 109%, 99%, 102%, 94%, 94%, 91%, 95% and 102%, respectively with a coefficient of variation below 6%. The method has been applied to the assessment of exposure in different areas of a farm and regarding the quantification of these compounds in the vapors generated by burning incense sticks and an essential oil marketed as air fresheners. The acquired results are comparable with those provided from a reference method for a 95% of confidence level. The possible use of these samplers for the sampling of other toxic compounds such as phthalates is evaluated by qualitative analysis of extracts from incense sticks and essential oil samples. Copyright © 2014 Elsevier B.V. All rights reserved.

  11. Determination of carbonyl compounds (acetaldehyde and formaldehyde in polyethylene terephthalate containers designated for water conservation

    Directory of Open Access Journals (Sweden)

    Redžepović Azra S.

    2012-01-01

    Full Text Available Polyethylene terephthalate (PET has in the last several years become the main packaging material for many food products, particularly carbonated beverages and bottled water, as well as for products of chemical industry (packaging of various hygiene maintenance agents, pesticides, solvents, etc.. The strength and permeability properties of PET are very good for packaging of beverages, its resistance to chemicals is high and it has a high degree of transparency. Acetaldehyde and formaldehyde are formed during the thermoforming of PET containers. After cooling, acetaldehyde and formaldehyde remain trapped in the walls of a PET bottle and may migrate into the water after filling and storage. Since there are no migration tests in Serbia prescribed for the determination of acetaldehyde and formaldehyde, the purpose of the paper is to test the quantitative contents of carbonyl compounds (acetaldehyde and formaldehyde in PET containers of different volumes, made by various manufacturers of bottled mineral carbonated and noncarbonated water, and exposed to different temperatures. In this study, the migration of acetaldehyde and formaldehyde from PET bottles into mineral carbonated and noncarbonated water was determined by high performance liquid chromatography. Taking into consideration that formaldehyde and acetaldehyde have no UV active or fluorescent group, the chromatography shall be preceded by derivatization in a closed system (due to a low boiling point of acetaldehyde and formaldehyde, which shall transform carbonyl compounds into UV active compounds.

  12. Determination of volatile compounds in grape distillates by solid-phase extraction and gas chromatography.

    Science.gov (United States)

    Lukić, Igor; Banović, Mara; Persurić, Dordano; Radeka, Sanja; Sladonja, Barbara

    2006-01-06

    Solid-phase extraction (SPE) procedure on octadecylsilica (C18) was developed for accumulation of volatile compounds from grape distillates. The procedure was optimised for final analysis by capillary gas chromatography. At mass concentrations in model solutions ranging from 0.1 to 50 mg/l solid-phase extraction recoveries of all analytes ranged from 69% for 2-phenylethanol to 102% for capric acid, with RSD values from 2 to 9%. SPE recoveries of internal standards to be added in the sample solution prior to extraction, higher alcohols 2-ethyl-1-hexanol and 1-undecanol, were 97 and 93%, respectively, with RSD values of 3%. Detection limits of analyzed compounds in model solutions ranged from 0.011 mg/l for isoamyl acetate to 0.037 mg/l for caproic acid. Method efficiency was tested in relation to acetic acid content, volume fraction of ethanol and possible matrix effects. A significant influence of matrix on SPE efficiency for geraniol, cis-2-hexen-1-ol and cis-3-hexen-1-ol was detected. For the same reason, 2-phenylethanol could not be determined by developed SPE method in samples of grape distillates. The developed solid-phase extraction method was successfully applied to determine the differences in volatile compound content in different grape distillates produced by the distillation of crushed, pressed and fermented grapes.

  13. Determination of the major phenolic compounds in pomegranate juices by HPLC−DAD−ESI-MS.

    Science.gov (United States)

    Gómez-Caravaca, Ana María; Verardo, Vito; Toselli, Moreno; Segura-Carretero, Antonio; Fernández-Gutiérrez, Alberto; Caboni, Maria Fiorenza

    2013-06-05

    Traditionally, pomegranate (Punica granatum L.) has been consumed as fresh fruit or as pomegranate juice. In this study, the main phenolic compounds of 12 pomegranate varieties and 5 pomegranate clones were determined by HPLC−DAD−ESI-MS. Two chromatographic methods with a fused-core C18 column and a classical HPLC system were developed. Thirteen anthocyanins and fourteen other phenolic compounds were determined in the pomegranate juices. As far as we are concerned, a new flavonol-glycoside, phellatin or its isomer amurensin, has been tentatively identified for the first time in pomegranate juices. Total phenolic content ranged from 580.8 to 2551.3 mg/L of pomegranate juice. Anthocyanins varied between 20 to 82% of total phenolic content. Flavonoids were 1.6-23.6% of total phenolic compounds, while phenolic acids and ellagitannins were in the range 16.4-65.8%. The five clones reported a phenolic content comparable with that of the other pomegranate samples.

  14. Rapid determination of phenolic compounds in water samples by alternating-current oscillopolarographic titration

    Institute of Scientific and Technical Information of China (English)

    XIAO Jun-ping; WANG Xue-feng; ZHOU Qing-xiang; FAN Xiao-yuan; SU Xian-fa; Bai Hua-hua; DUAN Hai-jing

    2007-01-01

    A rapid, simple and sensitive method was demonstrated for the determination of phenolic compounds in water samples by alternating-current oscillopolarographic titration. With the presence of sulfuric acid, phenol could be transferred into a nitroso-compound by reacting with NaNO2. The titration end-point was obtained by the formation of a sharp cut in the oscillopolarographic with infinitesimal NaNO2 on double platinum electrodes. The results showed that phenol had an excellent linear relationship over the range of 4.82×10-6 -9.65×10-3 mol/L, the RSD of the proposed method was lower than 1.5%, and the spiked recoveries of three real water samples were in the range of 95.6%-106.9%.

  15. Determination of one-dimensional distribution of 14C-labelled compounds

    International Nuclear Information System (INIS)

    Rexa, R.; Kron, I.; Kralik, P.; Tykva, R.

    1988-01-01

    Three methods used for the determination of one-dimensional distribution of 14 C-labelled compounds are compared: measurement with position-sensitive detector (LB 282/511), liquid scintillation counting (LSC), and autoradiography with densitometric quantification. For a mutual comparison of these methods samples of blood serum were used, in which the fractional esterification rate (FER) was determined by means of LCAT Test. The agreement of the methods of FER determination on the basis of the measurement with LB 282/511 or LSC was checked. In the case of autoradiography a correction for non-linearity between the blackening and the number of β-particles striking the area unit was necessary. (author) 5 refs.; 5 figs

  16. [Determination of flavor compounds in foxtail millet wine by gas chromatography-mass spectrometry coupled with headspace solid phase microextraction].

    Science.gov (United States)

    Liu, Jingke; Zhang, Aixia; Li, Shaohui; Zhao, Wei; Zhang, Yuzong; Xing, Guosheng

    2017-11-08

    To comprehensively understand flavor compounds and aroma characteristics of foxtail millet wine, extraction conditions were optimized with 85 μm polyacrylate (PA), 100 μm polydimethylsiloxane (PDMS), 75 μm carboxen (CAR)/PDMS and 50/30 μm divinylbenzene (DVB)/CAR/PDMS fibers. The flavor compounds in foxtail millet wine were investigated by gas chromatography-mass spectrometry (GC-MS) coupled with headspace solid phase microextraction (HS-SPME), and the odor characteristics and intensity were analyzed by odor active values (OAVs). The samples of 8 mL were placed in headspace vials with 1.5 g NaCl, then the headspace vials were heated at 60℃ for 40 min. Using HS-SPME with different fibers, a total of 55 flavor compounds were identified from the samples, including alcohols, esters, benzene derivatives, hydrocarbons, acids, aldehydes, ketones, terpenes, phenols and heterocycle compounds. The main flavor compounds were alcohols compounds. According to their OAVs, phenylethyl alcohol, styrene, 1-methyl-naphthalene, 2-methyl-naphthalene, benzaldehyde, benzeneacetaldehyde and 2-methoxy-phenol were established to be odor-active compounds. Phenylethyl alcohol and benzeneacetaldehyde were the most prominent odor-active compounds. PA and PDMS fibers had good extraction effect for polar and nonpolar compounds, respectively. CAR/PDMS and DVB/CAR/PDMS provided a similar compounds profile for moderate polar compounds. This research comprehensively determined flavor compounds of foxtail millet wine, and provided theoretical basis for product development and quality control.

  17. Analytical applications of oscillatory chemical reactions: determination of some pharmaceuticaly and biologically important compounds

    Directory of Open Access Journals (Sweden)

    Pejić Nataša D.

    2012-01-01

    Full Text Available Novel analytical methods for quantitive determination of analytes based on perturbations of oscillatory chemical reactions realized under open reactor conditions (continuosly fed well stirred tank reactor, CSTR, have been developed in the past twenty years. The proposed kinetic methods are generally based on the ability of the analyzed substances to change the kinetics of the chemical reactions matrix. The unambiguous correlation of quantitative characteristics of perturbations, and the amount (concentration of analyte expressed as a regression equation, or its graphics (calibration curve, enable the determination of the unknown analyte concentration. Attention is given to the development of these methods because of their simple experimental procedures, broad range of linear regression ( 10-7 10-4 mol L-1 and low limits of detection of analytes ( 10-6 10-8 mol L1, in some cases even lower than 10-12 mol L-1. Therefore, their application is very convenient for routine analysis of various inorganic and organic compounds as well as gases. This review summarizes progress made in the past 5 years on quantitative determination of pharmaceutically and biologically important compounds.

  18. Determination of the number of and classification of two-component ionic-covalent chemical compounds

    International Nuclear Information System (INIS)

    Vigdorovich, V.N.; Dzhuraev, T.D.; Khanin, V.A.

    1989-01-01

    The aim of this work was to determine the number of and to classify two-component compounds corresponding to the four-electron and full-valence concepts and characterized by the ionic-covalent type of bond, on which the metallic bond is superimposed to a greater lesser degree. At the same time it was proposed to verify the position of the axes in the periodic system. The presence of numerous compound analogs for the element prototypes of one axis of the Mendeleev periodic system [the group of noble (inert) gases] was confirmed by computer experiments. However, the other axis (the carbon group) is not so obvious and is evidently due, on account of the superimposition of the effect of noncharacteristic (possible) valences, to the elements of various groups (boron, aluminum, germanium, antimony, bismuth). In addition, the compound analogs for the element prototypes of the d block are numerous, i.e., the copper-silver-gold, manganese-technetium-rhenium, and iron and platinum families

  19. Quantitative Determination of Compounds from Akebia quinata by High-Performance Liquid Chromatography

    International Nuclear Information System (INIS)

    Yen, Nguyen; Thu, Nguyen; Zhao, Bing Tian; Woo, Mi Hee; Min, Byung Sun; Lee, Jae Hyun; Kim, Jeong Ah; Son, Jong Keun; Choi, Jae Sui; Woo, Eun Rhan

    2014-01-01

    To provide the scientific corroboration of the traditional uses of Akebia quinata (Thunb.) Decne., a detailed analytical examination of A. quinata stems was carried out using a reversed-phase high performance liquid chromatography (RP-HPLC) method coupled to photodiode array detector (PDA) for the simultaneous determination of four phenolic substances; cuneataside D, 2-(3,4-dihydroxyphenyl)ethyl-O-β-D-glucopyranoside, 3-caffeoylquinic acid and calceolarioside B. Particular attention was focused on the main compound, 3-caffeoylquinic acid, which has a range of biological functions. In addition, 2-(3,4-dihydroxyphenyl)ethyl-O-β-D-glucopyranoside was considered as a discernible marker of A. quinata from its easy confuse plants. The contents of compounds 2 and 3 ranged from 0.72 to 2.68 mg/g and from 1.66 to 5.64 mg/g, respectively. The validation data indicated that this HPLC/PDA assay was used successfully to quantify the four phenolic compounds in A. quinata from different locations using relatively simple conditions and procedures. The pattern-recognition analysis data from 53 samples classified them into two groups, allowing discrimination between A. quinata and comparable herbs. The results suggest that the established HPLC/PDA method is suitable for quantitation and pattern-recognition analyses for a quality evaluation of this medicinal herb

  20. Quantitative Determination of Compounds from Akebia quinata by High-Performance Liquid Chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Yen, Nguyen; Thu, Nguyen; Zhao, Bing Tian; Woo, Mi Hee; Min, Byung Sun [Catholic Univ. of Daegu, Gyeongsan (Korea, Republic of); Lee, Jae Hyun [Dongguk Univ., Yongin (Korea, Republic of); Kim, Jeong Ah [Kyungpook National Univ., Daegu (Korea, Republic of); Son, Jong Keun [Yeungnam Univ., Gyeongsan (Korea, Republic of); Choi, Jae Sui [Pukyung National Univ., Busan (Korea, Republic of); Woo, Eun Rhan [Chosun Univ., Gwangju (Korea, Republic of)

    2014-07-15

    To provide the scientific corroboration of the traditional uses of Akebia quinata (Thunb.) Decne., a detailed analytical examination of A. quinata stems was carried out using a reversed-phase high performance liquid chromatography (RP-HPLC) method coupled to photodiode array detector (PDA) for the simultaneous determination of four phenolic substances; cuneataside D, 2-(3,4-dihydroxyphenyl)ethyl-O-β-D-glucopyranoside, 3-caffeoylquinic acid and calceolarioside B. Particular attention was focused on the main compound, 3-caffeoylquinic acid, which has a range of biological functions. In addition, 2-(3,4-dihydroxyphenyl)ethyl-O-β-D-glucopyranoside was considered as a discernible marker of A. quinata from its easy confuse plants. The contents of compounds 2 and 3 ranged from 0.72 to 2.68 mg/g and from 1.66 to 5.64 mg/g, respectively. The validation data indicated that this HPLC/PDA assay was used successfully to quantify the four phenolic compounds in A. quinata from different locations using relatively simple conditions and procedures. The pattern-recognition analysis data from 53 samples classified them into two groups, allowing discrimination between A. quinata and comparable herbs. The results suggest that the established HPLC/PDA method is suitable for quantitation and pattern-recognition analyses for a quality evaluation of this medicinal herb.

  1. Method for determining the composition of the sugar moiety of a sugar containing compound

    DEFF Research Database (Denmark)

    2016-01-01

    The present invention relates to methods of labeling sugar moieties of sugar containing compounds including glycopeptides. The compounds presented in the present invention facilitate reliable detection of sugar moieties of sugar containing compounds by a combination of spectroscopy methods...

  2. Spectrographic determination of zirconium, niobium, rhodium, ruthenium, tantalum, and tungsten in uranium and its compounds

    International Nuclear Information System (INIS)

    Alduan, F.A.; Capdevila, C.

    1976-01-01

    The determination of Nb, Rh, Ru, Ta, W and Zr in uranium and its compounds has been studied, using the carrier distillation method with either AgCl or AgCl-SrF 2 (4:3) as carrier. In order to get the best sensitivity, the influence of the carrier concentration, the dc arc intensity and several controlled atmospheres on the variation of the line to background ratio of intensities has been considered. With the most suitable conditions, the sensitivities achieved for the considered elements are in the range 1-10 ppm. (author)

  3. Determination of carbonyl compounds in air by HPLC; Determinacion de compuestos carbonilicos en aire por HPLC

    Energy Technology Data Exchange (ETDEWEB)

    Garcia, S; Perez, R M; Campos, A; Gonzalez, D

    1995-07-01

    A method for the determination of seven carbonyl compounds in air is presented. The procedure involve sampling of air by a Sep-Pak Cartridge impregnated with 2,4-dinitrophenylhydrazine. Elution was done with 3 mL of acetonitrile and the eluate was diluted to 5 mL. The analysis was done by HPLC with UV detection and external standard method quantification. It has been achieved relative standard deviations about 5% and detection limits of 80 ng/cartridge for formaldehyde, acetaldehyde and acetoacetonitrile. Three different types of samples (rural, urban, petrol emission) were successfully analyzed. (Author) 12 refs.

  4. Chromatographic methods for determination of metals as chelate compounds with heterocyclic azo reagents

    International Nuclear Information System (INIS)

    Basova, E.M.; Bol'shova, T.A.; Shpigun, O.A.; Ivanov, V.M.

    1993-01-01

    Methods for separation and concentration of transition metals as well as cadmium in form of chelates with heterocyclic azo compounds namely, PAN(1-(2-pyridylaso)-2-naphthol), PAR(4-(2-pyridylazo)-resorcin), Br-PAAP (2-(5-bromine-2-pyridylazo)-5-diethyl aminophenol) are considered. The Br-PAAP reagent is the most sensitive and widely-applied one in extraction and highly-efficient liquid chromatography. Methods of sorption concentration with subsequent element determination directly on the sorbent without microelements separation or destruction are the most promissing ones

  5. DETERMINATION OF CHLORINATED ORGANIC COMPOUNDS IN THE MAIN DRAINAGE CHANNEL OF KONYA

    Directory of Open Access Journals (Sweden)

    Mehmet Emin AYDIN

    2000-03-01

    Full Text Available The main drainage channel of Konya collects drainage waters from farmlands of Konya and discharges to the salt lake. Since there is not any city municipal sewarage system in Konya sewage of the city also discharged to the main drainage channel. Along the channel, farmers use the channels water for irrigation purposes. Therefore a through examination of wastewater and determination of chlorinated compounds were necessary. In this research, analyses were carried by gas chromatography (GC on water samples collected hourly, daily and monthly from the channel.

  6. Flame photometric determination of Na, K and Li in uranium compounds

    International Nuclear Information System (INIS)

    Sabato, S.F.; Lordello, A.R.

    1985-01-01

    A flame photometric method for the determination of Na, K and Li in uranium compounds is described. The uranium is separated by solvent extraction from hydrochloric acid medium with tri-butyl phosphate. Amounts of uranium in order of 20 μg/ml don't cause any interference in the photometric results. The element Na presents a residual concentration due to the contamination of the reagents. The relative standard deviation is about 10% for the three elements. The relative error varies with the concentration of the element and it is between 1 and 24% for Na, between O and 12% for K and between O and 33% for Li. (Author) [pt

  7. Determination of chlorine in nuclear-grade uranium compounds by ion-selective electrode

    International Nuclear Information System (INIS)

    Yang Chunqing; Liu Fuyun; Huang Dianfan.

    1989-01-01

    The determination of microamount chlorine in nuclear-grade uranium compounds is described. Chlorine is separated from uranium oxide pyrohydrolytically with stream of wet oxygen in a furnace at 800-900 deg C. Chlorine is volatilized as hydrochloric acid, which then is absorbed in a dilute alkaline solution and measured with chlorine selective electrode. This method covers the concentration range of 10-500 ppm chlorine in uranium oxide. The relative standard diviation is better than 10% and recovery of 85-108% has been reported

  8. Determination of arsenenic compounds in environmental and biological samples with LAMMA and HPLC-ICP-MS

    International Nuclear Information System (INIS)

    Goessler, W.

    1997-07-01

    Different arsonium salts and alkyl- or aryl arsine sulfides were analyzed with a Laser-Microprobe-Mass-Analyzer (LAMMA-500). The positive-ion spectra of the arsonium salts showed clear signals for the (CH 3 ) 3 AsR + fragment. In the positive-ion spectra of alkyl- or arylarsine sulfides these arsenic compounds the molecular ions R 3 AsS + were never observed, but in most of the spectra the protonated parent compounds R 3 AsSH2 + were present. The negative-ion spectra showed mainly fragments S-n (n = 1, 2, 3, 4) and AsS n (n = 1, 2, 3). Chlorella vulgaris Beijerinck var. vulgaris with a concentration of 13,000 mg As/kg dry mass were analyzed with the LAMMA-500 to identify arsenic compounds. Surprisingly, arsenic could not be detected by the LAMMA technique at these high arsenic concentrations. Electron microscopy of Chlorella cells reveals, that particles adhered at the surface of the cells. Scanning transmission electron microscopy showed a high correlation between the arsenic concentration and the iron concentration in these particles. Algae may protect themselves from high arsenic concentrations, by precipitating FeAsO 4 at the cell surface. Different Chlorella sp. were grown to investigate the arsenic tolerance of Chlorella strains. Chlorella Boehm and Chlorella Kessleri grew better in arsenic-containing than in arsenic-free media. The growth of Chlorella 108 was depressed in high-arsenic media. After harvesting, the algal biomass was extracted and arsenic compounds determined in the extracts with HPLC-ICP-MS. Approximately 98 % of the total arsenic were present as arsenic acid. A method for the simultaneous identification and quantification of arsenocholine, arsenous acid, dimethylarsinic acid, arsenobetaine, methylarsonic acid, and arsenic acid at concentrations below 1 μg/L was developed. The developed HPLC-MPN-ICP-MS system allows the determination of arsenic compounds in urine sample at concentrations of 0.5 μg As/L with a relative standard deviation of

  9. How to tackle chemical communication? Relative proportions versus semiquantitative determination of compounds in lizard chemical secretions.

    Science.gov (United States)

    García-Roa, Roberto; Sáiz, Jorge; Gómara, Belén; López, Pilar; Martín, José

    2018-02-01

    Knowledge about chemical communication in some vertebrates is still relatively limited. Squamates are a glaring example of this, even when recent evidences indicate that scents are involved in social and sexual interactions. In lizards, where our understanding of chemical communication has considerably progressed in the last few years, many questions about chemical interactions remain unanswered. A potential reason for this is the inherent complexity and technical limitations that some methodologies embody when analyzing the compounds used to convey information. We provide here a straightforward procedure to analyze lizard chemical secretions based on gas chromatography coupled to mass spectrometry that uses an internal standard for the semiquantification of compounds. We compare the results of this method with those obtained by the traditional procedure of calculating relative proportions of compounds. For such purpose, we designed two experiments to investigate if these procedures allowed revealing changes in chemical secretions 1) when lizards received previously a vitamin dietary supplementation or 2) when the chemical secretions were exposed to high temperatures. Our results show that the procedure based on relative proportions is useful to describe the overall chemical profile, or changes in it, at population or species levels. On the other hand, the use of the procedure based on semiquantitative determination can be applied when the target of study is the variation in one or more particular compounds of the sample, as it has proved more accurate detecting quantitative variations in the secretions. This method would reveal new aspects produced by, for example, the effects of different physiological and climatic factors that the traditional method does not show.

  10. Comparison of mild extraction procedures for determination of plant-available arsenic compounds in soil

    Energy Technology Data Exchange (ETDEWEB)

    Szakova, Jirina; Tlustos, Pavel; Pavlikova, Daniela; Balik, Jiri [Czech University of Agriculture, Department of Agrochemistry and Plant Nutrition, Prague (Czech Republic); Goessler, Walter; Schlagenhaufen, Claudia [Karl-Franzens-University Graz, Institute of Chemistry, Analytical Chemistry, Graz (Austria)

    2005-05-01

    In this work three mild extraction agents for determination of plant-available fractions of elements in soil were evaluated for arsenic speciation in soil samples. Pepper (Capsicum annum, L.) var. California Wonder was cultivated in pots, and aqueous solutions of arsenite, arsenate, methylarsonic acid, and dimethylarsinic acid, at a concentration of 15 mg As kg{sup -1} soil, were added at the beginning of the experiment. Control pots (untreated) were also included. Deionized water, 0.01 mol L{sup -1} CaCl{sub 2}, and 0.05 mol L{sup -1} (NH{sub 4}){sub 2}SO{sub 4} were used to extract the plant-available fraction of the arsenic compounds in soil samples collected during the vegetation period of the plants. Whereas in control samples the extractable arsenic fraction did not exceed 1% of total arsenic content, soil amendment by arsenic compounds resulted in extraction of larger amounts, which varied between 1.4 and 8.1% of total arsenic content, depending on soil treatment and on the extracting agent applied. Among arsenic compounds determined by HPLC-ICPMS arsenate was predominant, followed by small amounts of arsenite, methylarsonic acid, and dimethylarsinic acid, depending on the individual soil treatment. In all the experiments in which methylarsonic acid was added to the soil methylarsonous acid was detected in the extracts, suggesting that the soil bacteria are capable of reducing methylarsonic acid before a further methylation occurs. No significant differences were observed between analytical data obtained by using different extraction procedures. (orig.)

  11. Simultaneous Determination of Florfenicol and Diclazuril in Compound Powder by RP-HPLC-UV Method

    Directory of Open Access Journals (Sweden)

    Leilei Guo

    2014-01-01

    Full Text Available A RP-HPLC-UV method was developed and validated for simultaneous determination of florfenicol and diclazuril in compound powder. The separation involved using a SinoChoom ODS-BP C18 (5 μm, 4.6 mm × 250 mm analytical column. The mobile phase was a mixture of acetonitrile-0.2% phosphoric acid (pH was adjusted to 3.0 with triethylamine. The ratio of acetonitrile and 0.2% phosphoric acid in the mobile phase was 60 : 40 (v/v from 0 minutes to 6 minutes and 70 : 30 (v/v from 6.1 minutes to 15 minutes. The flow rate was 1 mL/min. The temperature of the analytical column was maintained at 30°C. The detection was monitored at 225 nm and 277 nm for florfenicol and diclazuril, respectively. The excipients in the compound powder did not interfere with the drug peaks. The calibration curves of florfenicol and diclazuril were fairly linear over the concentration ranges between 50.0–500.0 μg/mL (r=0.9995 and 10.0–100.0 μg/mL (r=0.9992, respectively. The RSD of both the intraday and interday variations was below 2.1% for florfenicol and diclazuril. The method was successfully validated according to International Conference on Harmonisation and proved to be suitable for the simultaneous determination of florfenicol and diclazuril in compound powder.

  12. Spectral determination of individual rare earths in different classes of inorganic compounds

    International Nuclear Information System (INIS)

    Karpenko, L.I.; Fadeeva, L.A.; Shevchenko, L.D.

    1979-01-01

    The conditions are found allowing to analyze various inorganic compounds for rare-earth elements without separation from non-rare-earth components. The influence of the plasma composition on the intensity of spectral lines of rare-earth elements is studied. The relative intensity of homologous spectral lines of various rare-earth elements remains constant regardless of the plasma composition. The conditions are found for the determination of individual rare-earth elements acting as both alloying additives (Csub(n) -- n x 10 -1 -n x 10 -3 %), and basic components (up to tens of per cent) in different classes of inorganic compounds of 1-7 elements. The general method is developed for the determination of individual rare-earth elements in mixtures of oxides of rare-earth elements, complex fluorides of rare-earth elements and elements of group 2, gallates, borates, germanates, vanadates of rare-earth elements and aluminium; zirconates-titanates of lead and barium, containing modifying additives of rare-earth elements, complex chalcogenides of rare-earth elements and elements of group 5

  13. Hard cap espresso extraction and liquid chromatography determination of bioactive compounds in vegetables and spices.

    Science.gov (United States)

    Martinez-Sena, María Teresa; de la Guardia, Miguel; Esteve-Turrillas, Francesc A; Armenta, Sergio

    2017-12-15

    A new analytical procedure, based on liquid chromatography with diode array and fluorescence detection, has been proposed for the determination of bioactive compounds in vegetables and spices after hard cap espresso extraction. This novel extraction system has been tested for the determination of capsaicin and dihydrocapsaicin from fresh chilli and sweet pepper, piperine from ground pepper, curcumin from turmeric and curry, and myristicin from nutmeg. Extraction efficiency was evaluated by using acetonitrile:water and ethanol:water mixtures. The proposed method allows the extraction of samples with 100mL of 60% (v/v) ethanol in water. The obtained limits of quantification for the proposed procedure ranged from 0.07 to 0.30mgg -1 and results were statistically comparable with those obtained by ultrasound assisted extraction. Hard cap espresso machines offer a fast, effective and quantitative tool for the extraction of bioactive compounds from food samples with an extraction time lower than 30s, using a global available and low cost equipment. Copyright © 2017 Elsevier Ltd. All rights reserved.

  14. Determination of volatile organic compounds responsible for flavour in cooked river buffalo meat

    Directory of Open Access Journals (Sweden)

    A. Di Luccia

    2010-02-01

    Full Text Available Flavour is an important consumer attractive that directly influences the success of food products on the market. The determination of odorous molecules and their identification allows to useful knowledge for producers to valorise their own products. Buffalo meat has a different chemical composition from pork and beef and requires some cautions in cooking and processing. This work aims at the identification of volatile molecules responsible for flavours in river buffalo meat. The determination was carried out by solid phase micro-extraction (SPME technique and analysed by gas chromatography coupled to mass spectrometry (GC-MS. The most relevant results were the higher odorous impact of buffalo meat and the higher content of sulphide compounds responsible for wild aroma respect to pork and beef. These results were obtained comparing the total area of peaks detected in every chromatogram. We have also found significant differences concerning the contents of pentadecane, 1-hexanol-2 ethyl, butanoic acid, furano-2-penthyl. The origin of volatile organic compounds and their influence on the river buffalo aromas were discussed.

  15. Levels, trends and determinants of organohalogen compounds in breast milk in the netherlands

    Energy Technology Data Exchange (ETDEWEB)

    Houweling, D. A.; Steentjes, G. M.; Van Dekken, A.; Baumann, R. A.; Hoogerbrugge, R.; Zeilmaker, M. J.

    2002-07-01

    Since 1968, human milk surveys have been performed in the Netherlands at five year intervals to study trends in human exposure to polychlorinated organic compounds (POCs). From 1988 onwards dioxin-like congeners were analysed. The most recent campaign was carried out in 1998. In the campaign of 1998, in addition to the levels and trends of POCs in breast milk, potential determinants of the levels of POXCs in breast milk (such as the age of the mother, body mass index (BMI) of the mother, smoking behaviour and dietary habits) were also studied. Previously we presented preliminary results of the analysis of 36 breast milk samples. here we present the results of the analysis of 193 breast milk samples and the analysis of potential determinants of POC levels in breast milk. (Author) 8 refs.

  16. Determination of phenolic compounds and evaluation of antioxidant capacity of Campomanesia adamantium leaves

    Energy Technology Data Exchange (ETDEWEB)

    Coutinho, I.D.; Coelho, R.G.; Honda, N.K.; Silva, J.R.M.; Cardoso, C.A.L. [Universidade Federal de Mato Grosso do Sul (UFMS), Campo Grande, MS (Brazil). Dept. de Quimica]. E-mail: claudia@uems.br; Kataoka, V.M.F. [Universidade Estadual de Mato Grosso do Sul, Dourados, MS (Brazil). Curso de Quimica; Vilegas, W. [UNESP, Araraquara, SP (Brazil). Dept. de Quimica Organica

    2008-10-15

    Five flavanones and three chalcones were isolated from Campomanesia adamantium Berg. (Myrtaceae) leaves. The contents of these compounds were determined by HPLC. The phenolic contents were also determined. The monitoring of the antioxidant activity was carried out by inhibition of peroxidation using the linoleic acid system and radical-scavenging (DPPH). The plants were collected from 4 distinct cities of the Mato Grosso do Sul State, Brazil. The different samples exhibited a range of 4.67-232.35 mg/g chalcones and 15.62-50.71 mg/g flavanones and phenolic contents of the 7.24-21.19 mg/g gallic acid. All extracts showed high antioxidant activity with a wide range of the radical-scavenging (DPPH) from 52.0 to 92.2 % and inhibition oxidation of linoleic acid from 14.6 to 94.2%. (author)

  17. Determination of phenolic compounds and evaluation of antioxidant capacity of Campomanesia adamantium leaves

    International Nuclear Information System (INIS)

    Coutinho, I.D.; Coelho, R.G.; Honda, N.K.; Silva, J.R.M.; Cardoso, C.A.L.; Kataoka, V.M.F.; Vilegas, W.

    2008-01-01

    Five flavanones and three chalcones were isolated from Campomanesia adamantium Berg. (Myrtaceae) leaves. The contents of these compounds were determined by HPLC. The phenolic contents were also determined. The monitoring of the antioxidant activity was carried out by inhibition of peroxidation using the linoleic acid system and radical-scavenging (DPPH). The plants were collected from 4 distinct cities of the Mato Grosso do Sul State, Brazil. The different samples exhibited a range of 4.67-232.35 mg/g chalcones and 15.62-50.71 mg/g flavanones and phenolic contents of the 7.24-21.19 mg/g gallic acid. All extracts showed high antioxidant activity with a wide range of the radical-scavenging (DPPH) from 52.0 to 92.2 % and inhibition oxidation of linoleic acid from 14.6 to 94.2%. (author)

  18. Determination of the n-octanol/water partition coefficients of weakly ionizable basic compounds by reversed-phase high-performance liquid chromatography with neutral model compounds.

    Science.gov (United States)

    Liang, Chao; Han, Shu-ying; Qiao, Jun-qin; Lian, Hong-zhen; Ge, Xin

    2014-11-01

    A strategy to utilize neutral model compounds for lipophilicity measurement of ionizable basic compounds by reversed-phase high-performance liquid chromatography is proposed in this paper. The applicability of the novel protocol was justified by theoretical derivation. Meanwhile, the linear relationships between logarithm of apparent n-octanol/water partition coefficients (logKow '') and logarithm of retention factors corresponding to the 100% aqueous fraction of mobile phase (logkw ) were established for a basic training set, a neutral training set and a mixed training set of these two. As proved in theory, the good linearity and external validation results indicated that the logKow ''-logkw relationships obtained from a neutral model training set were always reliable regardless of mobile phase pH. Afterwards, the above relationships were adopted to determine the logKow of harmaline, a weakly dissociable alkaloid. As far as we know, this is the first report on experimental logKow data for harmaline (logKow = 2.28 ± 0.08). Introducing neutral compounds into a basic model training set or using neutral model compounds alone is recommended to measure the lipophilicity of weakly ionizable basic compounds especially those with high hydrophobicity for the advantages of more suitable model compound choices and convenient mobile phase pH control. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. The chemical nature of phenolic compounds determines their toxicity and induces distinct physiological responses in Saccharomyces cerevisiae in lignocellulose hydrolysates

    Science.gov (United States)

    2014-01-01

    We investigated the severity of the inhibitory effects of 13 phenolic compounds usually found in spruce hydrolysates (4-hydroxy-3-methoxycinnamaldehyde, homovanilyl alcohol, vanillin, syringic acid, vanillic acid, gallic acid, dihydroferulic acid, p-coumaric acid, hydroquinone, ferulic acid, homovanillic acid, 4-hydroxybenzoic acid and vanillylidenacetone). The effects of the selected compounds on cell growth, biomass yield and ethanol yield were studied and the toxic concentration threshold was defined for each compound. Using Ethanol Red, the popular industrial strain of Saccharomyces cerevisiae, we found the most toxic compound to be 4-hydroxy-3-methoxycinnamaldehyde which inhibited growth at a concentration of 1.8 mM. We also observed that toxicity did not generally follow a trend based on the aldehyde, acid, ketone or alcohol classification of phenolic compounds, but rather that other structural properties such as additional functional groups attached to the compound may determine its toxicity. Three distinctive growth patterns that effectively clustered all the compounds involved in the screening into three categories. We suggest that the compounds have different cellular targets, and that. We suggest that the compounds have different cellular targets and inhibitory mechanisms in the cells, also compounds who share similar pattern on cell growth may have similar inhibitory effect and mechanisms of inhibition. PMID:24949277

  20. Analysis of volatile organic compounds in compost samples: A potential tool to determine appropriate composting time.

    Science.gov (United States)

    Zhu, Fengxiang; Pan, Zaifa; Hong, Chunlai; Wang, Weiping; Chen, Xiaoyang; Xue, Zhiyong; Yao, Yanlai

    2016-12-01

    Changes in volatile organic compound contents in compost samples during pig manure composting were studied using a headspace, solid-phase micro-extraction method (HS-SPME) followed by gas chromatography with mass spectrometric detection (GC/MS). Parameters affecting the SPME procedure were optimized as follows: the coating was carbon molecular sieve/polydimethylsiloxane (CAR/PDMS) fiber, the temperature was 60°C and the time was 30min. Under these conditions, 87 compounds were identified from 17 composting samples. Most of the volatile components could only be detected before day 22. However, benzenes, alkanes and alkenes increased and eventually stabilized after day 22. Phenol and acid substances, which are important factors for compost quality, were almost undetectable on day 39 in natural compost (NC) samples and on day 13 in maggot-treated compost (MC) samples. Our results indicate that the approach can be effectively used to determine the composting times by analysis of volatile substances in compost samples. An appropriate composting time not only ensures the quality of compost and reduces the loss of composting material but also reduces the generation of hazardous substances. The appropriate composting times for MC and NC were approximately 22days and 40days, respectively, during the summer in Zhejiang. Copyright © 2016 Elsevier Ltd. All rights reserved.

  1. Competition between intermolecular interaction and configuration entropy as the structure-determining factor for inclusion compounds

    Energy Technology Data Exchange (ETDEWEB)

    Subbotin, O.; Belosludov, V.; Adamova, T. [Russian Academy of Science, Novosibirsk (Russian Federation). Nikolaev Inst. of Inorganic Chemistry; Belosludov, R.; Kawazoe, Y. [Tohoku Univ., Aoba-ku, Sendai (Japan). Inst. for Materials Research; Kudoh, J.I. [Tohoku Univ., Aoba-ku, Sendai (Japan). Center for Northeast Asia Studies

    2008-07-01

    This paper presented a newly developed method to accurately predict the thermodynamic properties of clathrate hydrates, particularly their structural phase transitions under pressure. The method is based on the theory of Van-der-Waals and Platteeuw with some modifications that include the influence of guest molecules on the host lattice. The model was used to explain the exception from the established rule that small guest molecules form structure s1 and large molecules form structure s2 hydrates. In this study, the thermodynamic properties of argon (Ar) hydrate and methane hydrate, each in both cubic structure s1 and s2 were modelled. The model showed that two competing factors play a role in the formation of inclusions, notably the intermolecular interaction of guest molecules with water molecules, and the configuration entropy. Competition of these 2 factors determines the structure of hydrate formed at different pressures. The model provides an accurate description of the thermodynamic properties of gas hydrates and how they behave under pressure. For the argon hydrates, the structural phase transition from structure s2 to s1 at high pressure was predicted, while methane hydrates were predicted to be metastable in the s2 structure. The model can be used for other inclusion compounds with the same type of composition such as clathrate silicon, zeolites, and inclusion compounds of semiconductor elements. 17 refs., 5 figs.

  2. In-tube extraction for the determination of the main volatile compounds in Physalis peruviana L.

    Science.gov (United States)

    Kupska, Magdalena; Jeleń, Henryk H

    2017-01-01

    An analytical procedure based on in-tube extraction followed by gas chromatography with mass spectrometry has been developed for the analysis of 24 of the main volatile components in cape gooseberry (Physalis peruviana L.) samples. According to their chemical structure, the compounds were organized into different groups: one hydrocarbon, one aldehyde, four alcohols, four esters, and 14 monoterpenes. By single-factor experiments, incubation temperature, incubation time, extraction volume, extraction strokes, extraction speed, desorption temperature, and desorption speed were determined as 60°C, 20 min, 1000 μL, 20, 50:50 μL/s, 280°C, 100 μL/s, respectively. Quantitative analysis using authentic standards and external calibration curves was performed. The limit of detection and limit of quantification for the analytical procedure were calculated. Results shown the benzaldehyde, ethyl butanoate, 2-methyl-1-butanol, 1-hexanol, 1-butanol, α-terpineol, and terpinen-4-ol were the most abundant volatile compounds in analyzed fruits (68.6-585 μg/kg). The obtained data may contribute to qualify cape gooseberry to the group of superfruits and, therefore, increase its popularity. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Syntheses and crystal structure determination by X-ray powder diffraction of new compounds of Benzovesamicol

    International Nuclear Information System (INIS)

    Rukiah, M.; Assaad, Th.

    2012-06-01

    The compound 2,2,2-Trifluoro-N-(1a,2,7,7 a-tetra-hydronaphtho[2,3-b]oxiren-3-yl)- acetamide, C 1 2H 1 0F 3 NO 2 , an important precursor in the preparation of benzovesamicol analogues for the diagnosis of Alzheimers disease, was prepared by the epoxidation of 5,8-dihydronaphthalene-1-amine using 3-chloroperoxybenzoic acid. The structure was determined by X-ray powder diffraction, multinuclear NMR spectroscopy and FT-IR spectroscopy. A pair of molecules form intermolecular N- H...O hydrogen bonds, involving the amino and oxirene groups, to produce a dimer.The two racemic compounds (2RS,3RS)-5-amino-3-(4-phenylpiperazin-1-yl)-1,2,3,4 tetrahydronaphthalene-2-ol, C 2 0H 2 5N 3 O, (I) and (2RS,3RS)-5-amino-3-[4-(3- methoxyphenyl)piperazin-1-yl]-1,2,3,4-tetrahydronaphthalene-2-ol, C 2 1H 2 7N 3 O 2 , (II) important benzovesamicol analogues for the diagnosis of Alzheimer's disease, have been synthesized and characterized by FT-IR, and 1 H and 13 C NMR spectroscopic analyses. The crystal structures were analyses using powder diffraction as no suitable single crystal were obtained. The two compounds are racemic mixtures of enantiomers which crystallize in the monoclinic system in a centrosymmetric space group (P21/c). Crystallography, in particular powder X-ray diffraction, was pivotal in revealing that the enantio-resolution did not succeed. In two compounds, the piperazine ring has a chair conformation, while the cyclohexene ring assumes a half-chair conformation. In (I) the crystal packing is mediated by weak contacts, principally by complementary intermolecular N--H...O hydrogen bonds that connect successive molecules into a chain. Further stabilization is provided by weak C--H...N contacts and by a weak intermolecular C--H...π interaction. While in (II), the crystal packing is dominated by intermolecular O--H...N hydrogen bonding which links molecules along the c direction. (authors)

  4. Determining inhibition effects of some aromatic compounds on peroxidase enzyme purified from white and red cabbage

    Energy Technology Data Exchange (ETDEWEB)

    Öztekin, Aykut, E-mail: aoztekin@agri.edu.tr [Ataturk University, Science Faculty, Department of Chemistry, 25240-Erzurum (Turkey); Agri Ibrahim Cecen University Faculty of Arts and Sciences, Department of Chemistry, 04100-Agri (Turkey); Almaz, Züleyha, E-mail: zturkoglu-2344@hotmail.com [Ataturk University, Science Faculty, Department of Chemistry, 25240-Erzurum (Turkey); Mus Alparslan University Faculty of Sciences, Department of Moleculer Biology, 49250-Mus (Turkey); Özdemir, Hasan, E-mail: hozdemir@atauni.edu.tr [Ataturk University, Science Faculty, Department of Chemistry, 25240-Erzurum (Turkey)

    2016-04-18

    Peroxidases (E.C.1.11.1.7) catalyze the one electron oxidation of wide range of substrates. They are used in synthesis reaction, removal of peroxide from industrial wastes, clinical biochemistry and immunoassays. In this study, the white cabbage (Brassica Oleracea var. capitata f. alba) and red cabbage (Brassica oleracea L. var. capitata f. rubra) peroxidase enzymes were purified for investigation of inhibitory effect of some aromatic compounds on these enzymes. IC{sub 50} values and Ki constants were calculated for the molecules of 6-Amino nicotinic hydrazide, 6-Amino-5-bromo nicotinic hydrazide, 2-Amino-5-hydroxy benzohydrazide, 4-Amino-3-hydroxy benzohydrazide on purified enzymes and inhibition type of these molecules were determined. (This research was supported by Ataturk University. Project Number: BAP-2015/98).

  5. Determining inhibition effects of some aromatic compounds on peroxidase enzyme purified from white and red cabbage

    Science.gov (United States)

    Öztekin, Aykut; Almaz, Züleyha; Özdemir, Hasan

    2016-04-01

    Peroxidases (E.C.1.11.1.7) catalyze the one electron oxidation of wide range of substrates. They are used in synthesis reaction, removal of peroxide from industrial wastes, clinical biochemistry and immunoassays. In this study, the white cabbage (Brassica Oleracea var. capitata f. alba) and red cabbage (Brassica oleracea L. var. capitata f. rubra) peroxidase enzymes were purified for investigation of inhibitory effect of some aromatic compounds on these enzymes. IC50 values and Ki constants were calculated for the molecules of 6-Amino nicotinic hydrazide, 6-Amino-5-bromo nicotinic hydrazide, 2-Amino-5-hydroxy benzohydrazide, 4-Amino-3-hydroxy benzohydrazide on purified enzymes and inhibition type of these molecules were determined. (This research was supported by Ataturk University. Project Number: BAP-2015/98).

  6. Determining inhibition effects of some aromatic compounds on peroxidase enzyme purified from white and red cabbage

    International Nuclear Information System (INIS)

    Öztekin, Aykut; Almaz, Züleyha; Özdemir, Hasan

    2016-01-01

    Peroxidases (E.C.1.11.1.7) catalyze the one electron oxidation of wide range of substrates. They are used in synthesis reaction, removal of peroxide from industrial wastes, clinical biochemistry and immunoassays. In this study, the white cabbage (Brassica Oleracea var. capitata f. alba) and red cabbage (Brassica oleracea L. var. capitata f. rubra) peroxidase enzymes were purified for investigation of inhibitory effect of some aromatic compounds on these enzymes. IC_5_0 values and Ki constants were calculated for the molecules of 6-Amino nicotinic hydrazide, 6-Amino-5-bromo nicotinic hydrazide, 2-Amino-5-hydroxy benzohydrazide, 4-Amino-3-hydroxy benzohydrazide on purified enzymes and inhibition type of these molecules were determined. (This research was supported by Ataturk University. Project Number: BAP-2015/98).

  7. Determination of 17 impurity elements in nuclear quality uranium compounds by atomic absorption spectroscopy

    International Nuclear Information System (INIS)

    Andonie, O.; Smith, L.A.; Cornejo, S.

    1985-01-01

    A method is described for the determination of 17 elements (Al, Ca, Cd, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Mo, Na, Ni, Pb, V and Zn) in the ppm level, in nuclearly pure uranium compounds by flame atomic absorption spectroscopy. The analysis is performed by first dissolving the uranium sample in nitric acid and then extracting the uranium with tributyl phosphate solution. The aqueous phase, free of uranium, which contains the elements to analyze is inspirated into the flame of an atomic absorption spectrophotometer using air-acetylene or nitrous oxide-acetylene flame according to the element in study. This method allows to extract the uranium selectively in more than 99.0% and the recovery of the elements sudied was larger 90% (for K) to 100% (for Cr). The sensitivity of the method vary from 0.096 μg/g U (for Cd) to 5.5 μg/g U (for Na). (Author)

  8. Non-Calorimetric Determination of the Adsorption Heat of Volatile Organic Compounds under Dynamic Conditions

    Directory of Open Access Journals (Sweden)

    Abdelhamid Korrir

    2015-04-01

    Full Text Available Avoiding strong chemical bonding, as indicated by lower heat of adsorption value, is among the selection criteria for Volatile Organic Compounds adsorbents. In this work, we highlight a non-calorimetric approach to estimating the energy of adsorption and desorption based on measurement of involved amounts, under dynamic conditions, with gaseous Fourier Transform Infrared spectroscopy. The collected data were used for obtaining adsorption heat values through the application of three different methods, namely, isosteric, temperature programmed desorption (TPD, and temperature-programmed adsorption equilibrium (TPAE. The resulting values were compared and discussed with the scope of turning determination of the heat of adsorption with non-calorimetric methods into a relevant decision making tool for designing cost-effective and safe operating of adsorption facilities.

  9. Indirect spectrophotometric determination of BIDA, DISIDA, DTPA and MDP in labelled compounds

    Energy Technology Data Exchange (ETDEWEB)

    Van der Walt, T.N.; Coetzee, P.P. (Rand Afrikaans Univ., Johannesburg (South Africa). Dept. of Chemistry); Fourie, P.J. (Atomic Energy Corp. of South Africa (Pty) Ltd., Pretoria (South Africa))

    1989-01-01

    N-(4-(n-butyl)acetanilide)iminodiacetic acid (BIDA), N-(2,6-diisopropylacetanilide)iminodiacetic acid (DISDA), diethylenetriaminepentaacetic acid (DTPA) and methylene diphosphonic acid (MDP) are used in labelling kits. The contents of BIDA, DISIDA or MDP of the {sup 99m}Tc-labelled compounds can be determined (indirectly) spectrophotometrically with copper, eriochrome cyanine R (ECC) and dodecyl-ethyldimethylammonium bromide (DEDA) in a sodium barbital buffered system at pH 8.5. The calibration curves obey Beer's Law from 0 to 40 {mu}g/25 mL for BIDA and DISIDA, 0 to 60 {mu}g/25 mL for DTPA and 0 to 100 {mu}g/10 mL for MDP. (author).

  10. Indirect spectrophotometric determination of BIDA, DISIDA, DTPA and MDP in labelled compounds

    International Nuclear Information System (INIS)

    Van der Walt, T.N.; Coetzee, P.P.

    1989-01-01

    N-(4-(n-butyl)acetanilide)iminodiacetic acid (BIDA), N-(2,6-diisopropylacetanilide)iminodiacetic acid (DISDA), diethylenetriaminepentaacetic acid (DTPA) and methylene diphosphonic acid (MDP) are used in labelling kits. The contents of BIDA, DISIDA or MDP of the 99m Tc-labelled compounds can be determined (indirectly) spectrophotometrically with copper, eriochrome cyanine R (ECC) and dodecyl-ethyldimethylammonium bromide (DEDA) in a sodium barbital buffered system at pH 8.5. The calibration curves obey Beer's Law from 0 to 40 μg/25 mL for BIDA and DISIDA, 0 to 60 μg/25 mL for DTPA and 0 to 100 μg/10 mL for MDP. (author)

  11. Field screening procedures for determining the presence of volatile organic compounds in soil

    International Nuclear Information System (INIS)

    Crockett, A.B.; DeHaan, M.S.

    1991-01-01

    Many field screening procedures have been used to detect the presence of volatile organic compounds (VOC) in soils but almost none have been documented and verified. Users of these procedures have not really known whether their objectives in screening were met. A reliable VOC screening procedure could significantly reduce the number of samples currently being submitted to laboratories, thereby reducing costs and improving site characterization. The Environmental Protection Agency's Environmental Monitoring Systems Laboratory in Las Vegas (EMSL-LV) has therefore sponsored a research effort to evaluate and improve headspace methods for screening soils for VOC in the field. The research involved comparing several extraction procedures using soils from actual waste sites, and determining the agitation and mixing necessary to achieve equilibrium. Headspace was analyzed using a relatively simple portable gas chromatograph with a short column. The results were variable and show that several procedures should be attempted and the results evaluated before selecting a screening procedure. 10 refs., 6 tabs

  12. Active machine learning-driven experimentation to determine compound effects on protein patterns.

    Science.gov (United States)

    Naik, Armaghan W; Kangas, Joshua D; Sullivan, Devin P; Murphy, Robert F

    2016-02-03

    High throughput screening determines the effects of many conditions on a given biological target. Currently, to estimate the effects of those conditions on other targets requires either strong modeling assumptions (e.g. similarities among targets) or separate screens. Ideally, data-driven experimentation could be used to learn accurate models for many conditions and targets without doing all possible experiments. We have previously described an active machine learning algorithm that can iteratively choose small sets of experiments to learn models of multiple effects. We now show that, with no prior knowledge and with liquid handling robotics and automated microscopy under its control, this learner accurately learned the effects of 48 chemical compounds on the subcellular localization of 48 proteins while performing only 29% of all possible experiments. The results represent the first practical demonstration of the utility of active learning-driven biological experimentation in which the set of possible phenotypes is unknown in advance.

  13. Exact Sight Distance Determination on Compound Vertical and Horizontal Curves in the Presence of Road Barriers

    Directory of Open Access Journals (Sweden)

    Chiu Liu, PhD, PE, PTOE

    2013-06-01

    Full Text Available The sight distance (SD on a three-dimensional (3-d compound curve has been studied recently in the absence of obstacles at road sides. Often, physical barriers are installed at road sides or in a roadway median for reducing potential collision severities; these rigid, semi-rigid, or even temporary cushion-type barriers can limit or reduce the driver's sight distance, depending on their horizontal offset distances away from the nearest edge of traveled way (ETW. The closer a barrier to the ETW is, the shorter the driver's sight distance would be. Since most barriers are constructed to prevent running-off road or crossing-median collisions, it is crucial to check whether the installation would reduce the driver's sight distance and potentially cause other traffic collisions such as rear-end or side swipe collisions. In this paper, an exact analytic framework is formulated with derived equations the first time to calculate the sight distance on a 3-d compound curve in the presence of a median barrier, a roadside barrier, or a temporary cushion or barrier used for construction or other maintenance purposes. This framework provides an engineer a handy tool to examine the possible change of SD in the presence of a barrier and choose the required horizontal offset/clearance of a barrier from the nearest traveled way edge to meet certain design criteria or standards. This critical offset distance determined using this framework not only reinforces the importance of having roadside clearance recovery zones on highways but also provides a method to determine its horizontal clearance from a different standpoint. This analytic framework can easily be programmed into an Excel spreadsheet to evaluate the design of a physical barrier and its potential influence on sight distance along a 3-d compound horizontal and vertical curve. Transportation engineers or practitioners may find this design tool handy and useful once the programmed spreadsheet is saved in a

  14. Extraction and determination of major hypotensive compounds in bark of Eucommia ulmoides Oliv.

    Directory of Open Access Journals (Sweden)

    Xiao Jianbo

    2009-01-01

    Full Text Available A reversed-phase liquid chromatographic method was developed for the quantitative determination of three major hypotensive compounds, namely geniposidic acid, chlorogenic acid, and geniposide in the bark of Eucommia ulmoides. Soxhlet extraction of GPA, GPS, and CA from E. ulmoides was optimized according to the Taguchi experimental design. Maximum global yields were obtained using the following conditions: extraction temperature, 80°C; extraction time, 1 h; number of extractions, three; solvent volume, 16 ml/g of sample; and 50% ethanol concentration in water. Optimal conditions of separation and detection were achieved on a Diamonsil ODS C18 column (150 mm × 4.6 mm, 5 μm with a linear gradient of methanol and 0.04% aqueous phosphoric acid (v/v at a flow rate of 1.0 ml/min and detection wavelength of 240 nm. All calibration curves showed good linearity (r2 > 0.999 within test ranges. The relative deviation of this method was less than 3% for intra- and inter-day assays, and the recovery percentage of the method was 95-104%, with a relative standard deviation (R.S.D. of less than 5%. The current assay method was used for quantitative determination of geniposidic acid, chlorogenic acid, and geniposide in five samples of E. ulmoides with different age. The results indicate that the developed method could be readily utilized as a quality control method in working with E. ulmoides.

  15. Simultaneous Determination of Eight Bioactive Compounds in Dianthus superbus by High-performance Liquid Chromatography.

    Science.gov (United States)

    Yun, Bo-Ra; Yang, Hye Jin; Weon, Jin Bae; Lee, Jiwoo; Eom, Min Rye; Ma, Choong Je

    2016-05-01

    Dianthus superbus, one of traditional herbal medicine, is widely used to treat urethritis, carbuncles and carcinoma. A simultaneous determination method was established for controlling the quality of D. superbus using the eight compounds, (E)-methyl-4-hydroxy-4-(8a-methyl-3-oxodecahydronaphthalen-4a-yl) (1), diosmetin-7-O(2'',6''-di-O-α-L-rhamnopyranosyl)-β-D-glucopyranoside (2), vanillic acid (3), 4-hydroxyphenyl acetic acid (4), 4-methoxyphenyl acetic acid (5), (E)-4-methoxycinnamic acid (6), 3-methoxy-4-hydroxyphenylethanol (7), and methyl hydroferulate (8) isolated from D. superbus. This analysis method was developed using high performance liquid chromatography coupled with diode array detector with a Shishedo C18 column at a column temperature of 3°C. The mobile phase was composed of 0.1% trifluoroacetic acid in water and acetonitrile. The flow rate was 1 ml/min and detection wavelength was set at 205 nm and 280 nm. Validation was performed in order to demonstrate selectivity, accuracy and precision of the method. The calibration curves showed good linearity (R (2) > 0.99). The limits of detection and limits of quantification were within the ranges 0.0159-0.6205 μg/ml and 0.3210-1.8802 μg/ml, respectively. Moreover, the relative standard deviations of intra- and inter-day precision were both Dianthus superbus was established by high performance liquid chromatography-diode array detectorDeveloped analysis method is validated with linearity, precious and accuracyThe newly established method was successfully evaluated contents of eight compounds in 12 D. superbus samples (D.1.D.12) from various regions and compared. Abbreviations used: HPLC: High performance liquid chromatography, LOD: Limits of detection, LOQ: Limits of quantification, RSD: Relative standard deviation.

  16. Position for determining gas-phase volatile organic compound concentrations in transuranic waste containers. Revision 2

    Energy Technology Data Exchange (ETDEWEB)

    Connolly, M.J.; Liekhus, K.J. [Lockheed Martin Idaho Technologies Co., Idaho Falls, ID (United States). Idaho National Engineering and Environmental Lab.; Djordjevic, S.M.; Loehr, C.A.; Spangler, L.R. [Benchmark Environmental Corp. (United States)

    1998-06-01

    In the conditional no-migration determination (NMD) for the test phase of the Waste Isolation Pilot Plant (WIPP), the US Environmental Protection Agency (EPA) imposed certain conditions on the US Department of Energy (DOE) regarding gas phase volatile organic compound (VOC) concentrations in the void space of transuranic (TRU) waste containers. Specifically, the EPA required the DOE to ensure that each waste container has no layer of confinement that contains flammable mixtures of gases or mixtures of gases that could become flammable when mixed with air. The EPA also required that sampling of the headspace of waste containers outside inner layers of confinement be representative of the entire void space of the container. The EPA stated that all layers of confinement in a container would have to be sampled until DOE can demonstrate to the EPA that sampling of all layers is either unnecessary or can be safely reduced. A test program was conducted at the Idaho National Engineering and Environmental Laboratory (INEEL) to demonstrate that the gas phase VOC concentration in the void space of each layer of confinement in vented drums can be estimated from measured drum headspace using a theoretical transport model and that sampling of each layer of confinement is unnecessary. This report summarizes the studies performed in the INEEL test program and extends them for the purpose of developing a methodology for determining gas phase VOC concentrations in both vented and unvented TRU waste containers. The methodology specifies conditions under which waste drum headspace gases can be said to be representative of drum gases as a whole and describes a method for predicting drum concentrations in situations where the headspace concentration is not representative. The methodology addresses the approach for determining the drum VOC gas content for two purposes: operational period drum handling and operational period no-migration calculations.

  17. Position for determining gas phase volatile organic compound concentrations in transuranic waste containers. Revision 1

    International Nuclear Information System (INIS)

    Connolly, M.J.; Liekhus, K.J.; Djordjevic, S.M.; Loehr, C.A.; Spangler, L.R.

    1995-08-01

    In the conditional no-migration determination (NMD) for the test phase of the Waste Isolation Pilot Plant (WIPP), the US Environmental Protection Agency (EPA) imposed certain conditions on the US Department of Energy (DOE) regarding gas phase volatile organic compound (VOC) concentrations in the void space of transuranic (TRU) waste containers. Specifically, the EPA required the DOE to ensure that each waste container has no layer of confinement that contains flammable mixtures of gases or mixtures of gases that could become flammable when mixed with air. The EPA also required that sampling of the headspace of waste containers outside inner layers of confinement be representative of the entire void space of the container. The EPA stated that all layers of confinement in a container would have to be sampled until DOE can demonstrate to the EPA that sampling of all layers is either unnecessary or can be safely reduced. A test program was conducted at the Idaho National Engineering Laboratory (INEL) to demonstrate that the gas phase VOC concentration in the void space of each layer of confinement in vented drums can be estimated from measured drum headspace using a theoretical transport model and that sampling of each layer of confinement is unnecessary. This report summarizes the studies performed in the INEL test program and extends them for the purpose of developing a methodology for determining gas phase VOC concentrations in both vented and unvented TRU waste containers. The methodology specifies conditions under which waste drum headspace gases can be said to be representative of drum gases as a whole and describes a method for predicting drum concentrations in situations where the headspace concentration is not representative. The methodology addresses the approach for determining the drum VOC gas content for two purposes: operational period drum handling and operational period no-migration calculations

  18. Position for determining gas-phase volatile organic compound concentrations in transuranic waste containers. Revision 2

    International Nuclear Information System (INIS)

    Connolly, M.J.; Liekhus, K.J.

    1998-06-01

    In the conditional no-migration determination (NMD) for the test phase of the Waste Isolation Pilot Plant (WIPP), the US Environmental Protection Agency (EPA) imposed certain conditions on the US Department of Energy (DOE) regarding gas phase volatile organic compound (VOC) concentrations in the void space of transuranic (TRU) waste containers. Specifically, the EPA required the DOE to ensure that each waste container has no layer of confinement that contains flammable mixtures of gases or mixtures of gases that could become flammable when mixed with air. The EPA also required that sampling of the headspace of waste containers outside inner layers of confinement be representative of the entire void space of the container. The EPA stated that all layers of confinement in a container would have to be sampled until DOE can demonstrate to the EPA that sampling of all layers is either unnecessary or can be safely reduced. A test program was conducted at the Idaho National Engineering and Environmental Laboratory (INEEL) to demonstrate that the gas phase VOC concentration in the void space of each layer of confinement in vented drums can be estimated from measured drum headspace using a theoretical transport model and that sampling of each layer of confinement is unnecessary. This report summarizes the studies performed in the INEEL test program and extends them for the purpose of developing a methodology for determining gas phase VOC concentrations in both vented and unvented TRU waste containers. The methodology specifies conditions under which waste drum headspace gases can be said to be representative of drum gases as a whole and describes a method for predicting drum concentrations in situations where the headspace concentration is not representative. The methodology addresses the approach for determining the drum VOC gas content for two purposes: operational period drum handling and operational period no-migration calculations

  19. A new method for determining gas phase heat of formation of aromatic energetic compounds

    Energy Technology Data Exchange (ETDEWEB)

    Keshavarz, Mohammad H. [Department of Chemistry, Malek-ashtar University of Technology, Shahin-shahr P. O. Box 83145/115 (Iran); Tehrani, Masoud K. [Department of Physics, Malek-ashtar University of Technology, Shahin-shahr P. O. Box 83145/115 (Iran)

    2007-04-15

    A new correlation is introduced for desk calculation of gas phase heat of formation of aromatic energetic compounds that contain the elements of carbon, hydrogen, nitrogen and oxygen. Predicted gas phase heats of formation for 26 energetic compounds have a root mean square of deviation from experiment of 20.67 kJ/mol, which is in good agreement with respect to measured values of oxygen-lean and oxygen-rich aromatic energetic compounds. (Abstract Copyright [2007], Wiley Periodicals, Inc.)

  20. Simultaneous determination of inorganic mercury and methylmercury compounds in natural waters

    Energy Technology Data Exchange (ETDEWEB)

    Logar, Martina; Horvat, Milena [Jozef Stefan Institute, Jamova 39, 1000 Ljubljana (Slovenia); Akagi, Hirokatsu [National Institute for Minamata Disease, 4058-18 Hama, Minamata, Kumamoto 867-0008 (Japan); Pihlar, Boris [Faculty of Chemistry and Chemical Technology, University of Ljubljana, Askerceva 5, 1000 Ljubljana (Slovenia)

    2002-11-01

    The purpose of the present work was to develop a simple, rapid, sensitive and accurate method for the simultaneous determination of inorganic mercury (Hg{sup 2+}) and monomethylmercury compounds (MeHg) in natural water samples at the pg L{sup -1} level. The method is based on the simultaneous extraction of MeHg and Hg{sup 2+}dithizonates into an organic solvent (toluene) after acidification of about 300 mL of a water sample, followed by back extraction into an aqueous solution of Na {sub 2}S, removal of H {sub 2}S by purging with N {sub 2}, subsequent ethylation with sodium tetraethylborate, room temperature precollection on Tenax, isothermal gas chromatographic separation (GC), pyrolysis and cold vapour atomic fluorescence spectrometric detection (CV AFS) of mercury. The limit of detection calculated on the basis of three times the standard deviation of the blank was about 0.006 ng L {sup -1} for MeHg and 0.06 ng L {sup -1} for Hg {sup 2+}when 300 mL of water was analysed. The repeatability of the results was about 5% for MeHg and 10% for Hg {sup 2+}. Recoveries were 90-110% for both species. (orig.)

  1. Reliable determination of new lipid peroxidation compounds as potential early Alzheimer Disease biomarkers.

    Science.gov (United States)

    García-Blanco, Ana; Peña-Bautista, Carmen; Oger, Camille; Vigor, Claire; Galano, Jean-Marie; Durand, Thierry; Martín-Ibáñez, Nuria; Baquero, Miguel; Vento, Máximo; Cháfer-Pericás, Consuelo

    2018-07-01

    Lipid peroxidation plays an important role in Alzheimer Disease, so corresponding metabolites found in urine samples could be potential biomarkers. The aim of this work is to develop a reliable ultra-performance liquid chromatography-tandem mass spectrometry analytical method to determine a new set of lipid peroxidation compounds in urine samples. Excellent sensitivity was achieved with limits of detection between 0.08 and 17 nmol L -1 , which renders this method suitable to monitor analytes concentrations in real samples. The method's precision was satisfactory with coefficients of variation around 5-17% (intra-day) and 8-19% (inter-day). The accuracy of the method was assessed by analysis of spiked urine samples obtaining recoveries between 70% and 120% for most of the analytes. The utility of the described method was tested by analyzing urine samples from patients early diagnosed with mild cognitive impairment or mild dementia Alzheimer Disease following the clinical standard criteria. As preliminary results, some analytes (17(RS)-10-epi-SC-Δ 15 -11-dihomo-IsoF, PGE 2 ) and total parameters (Neuroprostanes, Isoprostanes, Isofurans) show differences between the control and the clinical groups. So, these analytes could be potential early Alzheimer Disease biomarkers assessing the patients' pro-oxidant condition. Copyright © 2018 Elsevier B.V. All rights reserved.

  2. Comparison of methods for determining volatile compounds in milk, cheese, and whey powder

    Science.gov (United States)

    Solid phase microextraction (SPME) and gas chromatography-mass spectrometry (GC-MS) are commonly used for qualitative and quantitative analysis of volatile compounds in various dairy products, but conditions have to be adjusted for optimal SPME release while not generating new compounds that are abs...

  3. Determination of volatile compounds by gas liquid chromatography in tropical fruit, guava (psidium guajav L.)

    International Nuclear Information System (INIS)

    Hussain, A.; Zeb-un-Nisa; Asi, M. R.; Ahmad, R.; Iqbal, Z.; Maqbool, A. B.

    2002-01-01

    Volatile flavor components from both white and pink guava fruits were collected using Likens-Nickerson concurrent Distillation Extraction method and were analyzed by GC/FID. In the essence collected by using likens-Nickerson concurrent distillation extraction apparatus, 23 compounds were present in white guava fruit, of which 11 compounds (furfural, alpha-pinene, trans-2-hexene-1-ol, 2-heptanone, benzaldehyde, hexyl acetate Beta-ionone, limonene, 2-nonanone, cinamyl acetate and octyl acetate) were identified. Similarly for pink guava fruit, 13 compounds out of 29 compounds were identified by comparing retention times of unknown with that of standard compounds and sniffing at the odour port. These were hexanal, furfural, 2-heptanone, benzaldehyde, methyl furfural hexyl acetate, beta-ionone, alpha-pinene, 2-nonanone, limonene, cinnamyl acetate, ethyl undecanoate and octyl acetate. (author)

  4. Determination of Polar Compounds in Guava Leaves Infusions and Ultrasound Aqueous Extract by HPLC-ESI-MS

    Directory of Open Access Journals (Sweden)

    Elixabet Díaz-de-Cerio

    2015-01-01

    Full Text Available Literature lacks publications about polar compounds content in infusion or guava leaves tea. Because of that, a comparison between different times of infusion and a conventional ultrasound aqueous extract was carried out. Several polar compounds have been identified by HPLC-ESI-MS and their antioxidant activity was evaluated by FRAP and ABTS assays. Four different classes of phenolic compounds (gallic and ellagic acid derivatives, flavonols, flavanones, and flavan-3-ols and some benzophenones were determined. The quantification results reported that the order, in terms of concentration of the classes of polar compounds in all samples, was flavonols > flavan-3-ols > gallic and ellagic acid derivatives > benzophenones > flavanones. As expected, the aqueous extract obtained by sonication showed the highest content in the compounds studied. Significative differences were noticed about the different times of infusion and five minutes was the optimal time to obtain the highest content in polar compounds using this culinary method. All the identified compounds, except HHDP isomers and naringenin, were positively correlated with antioxidant activity.

  5. [Determination of organotin compounds in plastic products by GC/MS after ethyl derivatization with sodium tetraethylborate].

    Science.gov (United States)

    Ohno, Hiroyuki; Suzuki, Masako; Nakashima, Shigehito; Aoyama, Taiki; Mitani, Kazunori

    2002-08-01

    A simultaneous determination method for 9 organotin compounds in polyvinyl chloride (PVC) and silicone products used as kitchen utensils and food packages was developed using ethyl derivatization with sodium tetraethylborate (NaBEt4). Organotin compounds were extracted with acetone-hexane (3:7) from the samples after acidification and the extract was filtered and concentrated at under 40 degrees C. After centrifugal separation, these compounds were derivatized with 2% NaBEt4 solution and determined by GC/MS. This method was applicable for simple routine analysis. Recoveries of spiked compounds were 49.1-118.1% for 3 PVC products and 88.8-102.2% for a siliconized paper. Monooctyltin, dioctyltin and trioctyltin compounds were found in all PVC food containers at the levels of 123-1,380 micrograms/g, 1,770-13,200 micrograms/g and 6.6-139 micrograms/g, respectively. They also were found in 3 gloves, 5 spouts, 1 hose and 5 pipes. Some PVC products contained monomethyltin, dimethyltin, trimethyltin, monobutyltin and dibutyltin compounds at the levels of 97.3-433 micrograms/g, 96.5-5,120 micrograms/g, 8.5-24.9 micrograms/g, 1.2-852 micrograms/g and 1.2-29.4 micrograms/g, respectively.

  6. [Evaluation of uncertainty for determination of tin and its compounds in air of workplace by flame atomic absorption spectrometry].

    Science.gov (United States)

    Wei, Qiuning; Wei, Yuan; Liu, Fangfang; Ding, Yalei

    2015-10-01

    To investigate the method for uncertainty evaluation of determination of tin and its compounds in the air of workplace by flame atomic absorption spectrometry. The national occupational health standards, GBZ/T160.28-2004 and JJF1059-1999, were used to build a mathematical model of determination of tin and its compounds in the air of workplace and to calculate the components of uncertainty. In determination of tin and its compounds in the air of workplace using flame atomic absorption spectrometry, the uncertainty for the concentration of the standard solution, atomic absorption spectrophotometer, sample digestion, parallel determination, least square fitting of the calibration curve, and sample collection was 0.436%, 0.13%, 1.07%, 1.65%, 3.05%, and 2.89%, respectively. The combined uncertainty was 9.3%.The concentration of tin in the test sample was 0.132 mg/m³, and the expanded uncertainty for the measurement was 0.012 mg/m³ (K=2). The dominant uncertainty for determination of tin and its compounds in the air of workplace comes from least squares fitting of the calibration curve and sample collection. Quality control should be improved in the process of calibration curve fitting and sample collection.

  7. Carbon transfer in soil - plant system. Molecular labelling utilization for determining rhizosphere compounds

    International Nuclear Information System (INIS)

    Leguay, J.J.

    2000-01-01

    The growing up of the bacteria developing in the rhizosphere of plants is dependent on the compounds exudation by plant roots. Even the bacterial genetics use has permitted to identify diverse functions involved in the process of the rhizosphere colonisation ( mobility, heterotrophic bacteria, growing rate, antibiotics production), there is a big delay in vegetal partners. To decrease this delay we tried to characterize the interactions between a plant model, Arabidopsis thaliana and the rhizosphere bacteria. An experimental device has been conceived for measuring the transfer of carbon issued from the photosynthesis to roots and soil. The exudation by roots has been studied. The analysis of rhizospheric compounds in situ pose some methodological problems, especially, the rhizospheric compounds must be extracted from the soil matrix. we suggest an analysis method of rhizospheric compound and of their dynamics. (F.M.)

  8. Ionization Potentials of Chemical Warfare Agents and Related Compounds Determined with Density Functional Theory

    National Research Council Canada - National Science Library

    Wright, J

    2000-01-01

    ...) agents at contaminated sites. Reported herein are theoretical ionization potentials for CW agents and their related compounds calculated using density functional theory at the B3LYP/6-311+G(2d,p) level of theory...

  9. Determination of heat purgeable and ambient purgeable volatile organic compounds in water by gas chromatography/mass spectrometry

    Science.gov (United States)

    Rose, Donna L.; Sandstrom, Mark W.; Murtagh, Lucinda K.

    2016-09-08

    Two new analytical methods have been developed by the U.S. Geological Survey (USGS) National Water Quality Laboratory (NWQL) that allow the determination of 37 heat purgeable volatile organic compounds (VOCs) (USGS Method O-4437-16 [NWQL Laboratory Schedule (LS) 4437]) and 49 ambient purgeable VOCs (USGS Method O-4436-16 [NWQL LS 4436]) in unfiltered water. This report documents the procedures and initial performance of both methods. The compounds chosen for inclusion in the methods were determined as having high priority by the USGS National Water-Quality Assessment (NAWQA) Program. Both methods use a purge-and-trap technique with gas chromatography/mass spectrometry. The compounds are extracted from the sample by bubbling helium through a 25-milliliter sample. For the polar and less volatile compounds, the sample is heated at 60 degrees Celsius, whereas the less polar and more volatile compounds are purged using a separate analytical procedure at ambient temperature. The compounds are trapped on a sorbent trap, desorbed into a gas chromatograph/mass spectrometer for separation, and then identified and quantified. Sample preservation is recommended for both methods by adding a 1:1 solution of hydrochloric acid (HCl [1:1]) to water samples to adjust the pH to 2. Analysis within 14 days from sampling is recommended.The heat purgeable method (USGS Method O-4437-16) operates with the mass spectrometer in the simultaneous full scan/selected ion monitoring mode. This method supersedes USGS Method O-4024-03 (NWQL LS 4024). Method detection limits (MDLs) for fumigant compounds 1,2-dibromoethane, 1,2-dichloropropane, 1,2,3-trichloropropane, chloropicrin, and 1,2-dibromo-3-chloropropane range from 0.002 to 0.010 microgram per liter (µg/L). The MDLs for all remaining heat purgeable VOCs range from 0.006 µg/L for tert-butyl methyl ether to 3 µg/L for alpha-terpineol. Calculated holding times indicate that 36 of the 37 heat purgeable VOCs are stable for a minimum of 14 days

  10. Determination of crystal structures by x-ray diffraction: applications to a lanthanide complex and a natural organic compound

    International Nuclear Information System (INIS)

    Miranda, J.M. de.

    1986-01-01

    The study fir determining crystal structures of the Ho (ReO sub(4)) sub(3) 4 TDTD 3 H sub(2) O complex and the natural organic compound C sub(14) H sub(16) O sub(6) by X-ray diffraction are presented. The experimental equipments are described in details. (M.C.K.)

  11. Study of the effect of surfactants on extraction and determination of polyphenolic compounds and antioxidant capacity of fruits extracts.

    Directory of Open Access Journals (Sweden)

    Reza Hosseinzadeh

    Full Text Available Micelle/water mixed solutions of different surface active agents were studied for their effectiveness in the extraction of polyphenolic compounds from various varieties of apples from west Azerbaijan province in Iran. The total content of polyphenolic compound in fruit extracts were determined using ferrous tartrate and Folin-Ciocalteu assays methods and chromatographic methods and compared with theme. High performance liquid chromatography is one of the most common and important methods in biochemical compound identification. The effect of pH, ionic strength, surfactant type, surfactant concentration, extraction time and common organic solvent in the apple polyphenolics extractions was studied using HPLC-DAD. Mixtures of surfactants, water and methanol at various ratios were examined and micellar-water solutions of Brij surfactant showed the highest polyphenol extraction efficiency. Optimum conditions for the extraction of polyphenolic compounds from apple occurred at 7 mM Brij35, pH 3. Effect of ionic strength on extraction was determined and 2% (W/V potassium Chloride was determined to be the optimum salt concentration. The procedure worked well with an ultrasound bath. Total antioxidant capacity also was determined in this study. The method can be safely scaled up for pharmaceutical applications.

  12. Radioisotopic determination methods of sulphur dispersion and sulphur blooming in rubber compounds

    International Nuclear Information System (INIS)

    Goraczka, W.; Koczorowska, E.

    1997-01-01

    It is well known that the concentration of sulphur in rubber compounds essentially effects the structure of the vulkanizate network. But there are no efficient and accurate methods to estimate the dispersion and migration (blooming) of curatives in raw rubber. In the work radioisotope methods have been analyzed to study the dispersion of curatives, physical and chemical processes in rubber and to optimize technical conditions of tire production. The radioactivity of the 35 S isotope introduced into rubber compounds has been measured by volumetric and surface methods. It was proved that the radioisotopic methods can be used in the studies. Experimental data of the effect of selected technological factors on these processes are presented. Rubber compounds containing soluble sulphur were made for such investigations. These methods permit detection of concentrations 10 -6 g of the radioactive isotope per 0.1 g of rubber compound. The sensitivity of these methods enables the investigation of radioisotope behaviour in rubber compounds during processing on an industrial scale without any hazards for workers

  13. Does lipophilicity of toxic compounds determine effects on drought tolerance of the soil collembolan Folsomia candida?

    International Nuclear Information System (INIS)

    Skovlund, Gitte; Damgaard, Christian; Bayley, Mark; Holmstrup, Martin

    2006-01-01

    The ability of Collembola to survive drought stress is crucial for their distribution in the terrestrial environment. Previous studies have suggested that several toxic compounds affect the drought tolerance of Folsomia candida in a synergistic manner and that these compounds have the feature in common that they elicit their toxicity by causing membrane damage. We hypothesised that the detrimental effect of toxic chemicals on drought tolerance in F. candida depends on the lipophilicity (log K ow ) of the compound because a higher log K ow would mean a closer interaction with membranes. In this study the three chemicals 4-nonylphenol, pyrene and p,p'-DDE were tested. Surprisingly, 4-nonylphenol, with the lowest log K ow , was the most potent with respect to reducing drought tolerance followed by pyrene, suggesting that interactions between drought tolerance and chemical stress do not depend on lipophilicity alone. - Toxic stress may reduce drought tolerance of Collembola

  14. Cytochrome c biosensor for determination of trace levels of cyanide and arsenic compounds

    International Nuclear Information System (INIS)

    Fuku, Xolile; Iftikar, Faiza; Hess, Euodia; Iwuoha, Emmanuel; Baker, Priscilla

    2012-01-01

    Highlights: ► Cytochrome c biosensor for detection of KCN, As 2 O 3 and Fe 2 K (CN) was constructed. ► Detection limits in the range of 4.3–9.1 μM for the analytes were obtained using CV, SWV and EIS. ► The detection limits for the biosensor were significantly lower than current EPA and WHO guidelines. - Abstract: An electrochemical method based on a cytochrome c biosensor was developed, for the detection of selected arsenic and cyanide compounds. Boron doped diamond (BDD) electrode was used as a transducer, onto which cytochrome c was immobilised and used for direct determination of Prussian blue, potassium cyanide and arsenic trioxide. The sensitivity as calculated from cyclic voltammetry (CV) and square wave voltammetry (SWV), for each analyte in phosphate buffer (pH = 7) was found to be in the range of (1.1–4.5) × 10 −8 A μM −1 and the detection limits ranged from 4.3 to 9.1 μM. The biosensor is therefore able to measure significantly lower than current Environmental Protection Agency (EPA) and World Health Organisation (WHO) guidelines, for these types of analytes. The protein binding was monitored as a decrease in biosensor peak currents by SWV and as an increase in biosensor charge transfer resistance by electrochemical impedance spectroscopy (EIS). EIS provided evidence that the electrocatalytic advantage of BDD electrode was not lost upon immobilisation of cytochrome c. The interfacial kinetics of the biosensor was modelled as equivalent electrical circuit based on electrochemical impedance spectroscopy data. UV–vis spectroscopy was used to confirm the binding of the protein in solution by monitoring the intensity of the soret bands and the Q bands. FTIR was used to characterise the protein in the immobilised state and to confirm that the protein was not denatured upon binding to the pre-treated bare BDD electrode. SNFTIR of cyt c immobilised at platinum electrode, was used to study the effect of oxidation state on the surface bond

  15. DETERMINATION OF PHASE COMPOSITION OF SEALING COATING BASED ON APC (ALUMINOPHOSPHATE COMPOUNDS

    Directory of Open Access Journals (Sweden)

    BOLSHAKOV V. I.

    2017-02-01

    Full Text Available Summary. Goal. To investigate the phase composition of the obtained sealing coatings based on aluminophosphate compound (APC and the impact of temperature rise on it. Methods. Qualitative X-ray phase analysis (XRPA and differential thermal analysis (DTA are used as the methods of research. Roentgenograms for structural analysis were obtained on a DRON-4-07 using filtered copper radiation in the secondary beam. Registration and initial processing of diffraction patterns was performed using the software package PDOS with the output of the diffraction patterns on the screen. Using the "loupe" option allowed to identify weak interference lines, which increased the accuracy of the method of qualitative XRPA. The thermograms for DTA received on the device type Termoskan-2. The results. It is revealed that base of coating is X-ray amorphous phase. There are following crystalline phases: Al, AlPO4, Al (PO3 3, BN found in the coating. It is revealed that annealing doesn’t make a significant influence on the phase composition of the crystalline phases and the coating doesn’t lose properties after annealing during repeated thermal stress. Scientific novelty. The phase composition of the proposed sealing coatings based on APC and produced by plasma spraying, and the effect of annealing on the phase composition of the coating are investigated. The reaction of synthesis of primary material forming on the basis of APC for coating is offered. Practical significance. The results can be used in aviation technology in the development of gas turbine engines (GTE and the design of the compressors. The sealing coating may be used to improve the reliability of the compressor and to increase the efficiency ratio of turbine engine. During the operation the compressor’s blades touch the sealing coating of compressor’s stator and grooves it without causing locking and destruction of the rotor. Therefore, the development of new sealing coating compositions that

  16. Determination of isotope ratio of elements by mass distribution in molecules of varied chemical compounds

    International Nuclear Information System (INIS)

    Gladkikh, I.S.; Babichev, A.P.

    1999-01-01

    The procedure and program for calculation of isotope ratio of elements involving in the compound being studied using data of mass spectrometry were elaborated. The methods developed for the O 2 , SiH 4 , Cd(CH 3 ) 2 molecules were demonstrated for the illustration. The results of calculation provide support for the efficiency of the program and satisfactory reliability of the results during calculation of the isotope and complex compound concentrations. The program may be used for the estimation of the degree of nonequilibrium isotope distributions, it may indicate on the errors of the mass spectroscopy results [ru

  17. Quantitative determination of secoiridoid and gamma-pyrone compounds in Gentiana lutea cultured in vitro.

    Science.gov (United States)

    Menković, N; Savikin-Fodulović, K; Momcilović, I; Grubisić, D

    2000-02-01

    The production of secondary metabolites was studied in shoots, roots, and hairy roots of Gentiana lutea obtained in vitro. In shoots, both secoiridoid and gamma-pyrone compounds were detected in amounts similar to those found in aerial parts of plants collected from nature. The most abundant secoiridoid was gentiopicrin while mangiferin was the main compound among the gamma-pyrones. The adventitious roots obtained in vitro showed a poor biosynthetic capacity. Upon infection with Agrobacterium rhizogenes, nine hairy root clones were established which differed in the amount of secondary metabolites.

  18. Determination of phenolic compounds using high-performance liquid chromatography with Ce4+-Tween 20 chemiluminescence detection

    International Nuclear Information System (INIS)

    Cui Hua; Zhou Jian; Xu Feng; Lai Chunze; Wan Guohui

    2004-01-01

    A novel method for the simultaneous determination of phenolic compounds such as salicylic acid, resorcinol, phloroglucinol, p-hydroxybenzoic acid, 2,4-dihydroxybenzoic acid, and m-nitrophenol by high-performance liquid chromatography (HPLC) coupled with chemiluminescence (CL) detection was developed. The procedure was based on the chemiluminescent enhancement by phenolic compounds of the cerium(IV)-Tween 20 system in a sulfuric acid medium. The separation was carried out with an isocratic elution or with a gradient elution using a mixture of methanol and 1.5% acetic acid. For six phenolic compounds, the detection limits (3σ) were in the range 1.40-5.02 ng/ml and the relative standard deviations (n=11) for the determination of 0.1 μg/ml compounds were in the range 1.9-2.9%. The CL reaction was well compatible with the mobile phase of HPLC, no baseline drift often occurred in HPLC-CL detection was observed with a gradient elution. The method has been successfully applied to the determination of salicylic acid and resorcinol in Dermatitis Clear Tincture and p-hydroxybenzoic acid in apple juices

  19. Self-propagating high temperature synthesis as a method of determination of formation heat of refractory compounds

    International Nuclear Information System (INIS)

    Maslov, V.M.; Neganov, A.S.; Borovinskaya, I.P.; Merzhanov, A.G.

    1978-01-01

    Determination possibility of formation heats of refractory compounds in the process of direct synthesis from elements in a special calorimeter in the combustion regime is studied. Determined are formation heats of carbides - ZrCsub(0.92), Hf Csub(0.93), TaCsub(0.86), borides - ZrB 2 , HfB 2 NbB, NbB 2 , TaB, TaB 2 , MoB and silicides - ZrSi, ZrSi 2 , MoSi 2 . The results of chemical and x-ray phase analyses of the synthesized compounds are also given. Total error of formation heat determination methods does not surpass 2.0%

  20. Analytical Procedure Development to Determine Polycyclic Aromatic Compounds in the PM2.5-PM10 Fraction of Atmospheric Aerosols

    International Nuclear Information System (INIS)

    Barrado, A. I.; Garcia, S.; Perez, R. M.

    2013-01-01

    This paper presents an optimized and validated analytical methodology for the determination of various polycyclic aromatic compounds in ambient air using liquid chromatography with fluorescence detection. This analysis method was applied to samples obtained during more than one year in an area of Madrid. Selected compounds have included thirteen polycyclic hydrocarbons considered priorities by the EPA, and hydroxylated derivatives, which have been less investigated in air samples by liquid chromatography with fluorescence detection. We have characterized and compared the concentration ranges of compounds identified and studied seasonal and monthly variations. In addition, the techniques have been applied to study multivariate correlations, factor analysis and cluster analysis to extract as much information as possible for interpretation and more complete and accurate characterization of the results and their relationship with meteorological parameters and physicochemical. (Author)

  1. Determination of dimethyl selenide and dimethyl sulphide compounds causing off-flavours in bottled mineral waters.

    Science.gov (United States)

    Guadayol, Marta; Cortina, Montserrat; Guadayol, Josep M; Caixach, Josep

    2016-04-01

    Sales of bottled drinking water have shown a large growth during the last two decades due to the general belief that this kind of water is healthier, its flavour is better and its consumption risk is lower than that of tap water. Due to the previous points, consumers are more demanding with bottled mineral water, especially when dealing with its organoleptic properties, like taste and odour. This work studies the compounds that can generate obnoxious smells, and that consumers have described like swampy, rotten eggs, sulphurous, cooked vegetable or cabbage. Closed loop stripping analysis (CLSA) has been used as a pre-concentration method for the analysis of off-flavour compounds in water followed by identification and quantification by means of GC-MS. Several bottled water with the aforementioned smells showed the presence of volatile dimethyl selenides and dimethyl sulphides, whose concentrations ranged, respectively, from 4 to 20 ng/L and from 1 to 63 ng/L. The low odour threshold concentrations (OTCs) of both organic selenide and sulphide derivatives prove that several objectionable odours in bottled waters arise from them. Microbial loads inherent to water sources, along with some critical conditions in water processing, could contribute to the formation of these compounds. There are few studies about volatile organic compounds in bottled drinking water and, at the best of our knowledge, this is the first study reporting the presence of dimethyl selenides and dimethyl sulphides causing odour problems in bottled waters. Copyright © 2016 Elsevier Ltd. All rights reserved.

  2. Determination of organotin compounds in the foodweb of a shallow freshwater lake in the Netherlands

    NARCIS (Netherlands)

    Stäb, J.A.; Traas, T.P.; Stroomberg, G.; van Kesteren, J.; Leonards, P.E.G.; van Hattum, A.G.M.; Brinkman, U.A.T.; Cofino, W.P.

    1996-01-01

    An extensive study on the presence of nine organotin compounds (OT) in a freshwater foodweb was made, using newly developed analytical procedures in order to obtain insight in accumulation and degradation processes. Tributyltin (TBT), Triphenyltin (TPT) and their degradation products were detected.

  3. Comparison of methods for determining volatile compounds in cheese, milk, and whey powder

    Science.gov (United States)

    Solid phase microextraction (SPME) and gas chromatography-mass spectrometry (GC-MS) are commonly used for qualitative and quantitative analysis of volatile compounds in various dairy products, but selecting the proper procedures presents challenges. Heat is applied to drive volatiles from the samp...

  4. Facile determination of the specific activity of carbonyl compounds reduced by tritiated borohydride

    Energy Technology Data Exchange (ETDEWEB)

    Avigad, G [Rutgers--the State Univ., Piscataway, NJ (USA)

    1979-12-01

    Three procedures are described for microliter samples of glucose 6-phosphate or lactose as model compounds. After the reduction with (/sup 3/H)-NaBH/sub 4/ and suitable treatment, specific activity is calculated from the ratios /sup 3/H activity/total phosphorus, /sup 3/H//sup 14/C activity, or /sup 3/H activity/galactoside concentration.

  5. Determination of Carbonyl Compounds in Cork Agglomerates by GDME-HPLC-UV: Identification of the Extracted Compounds by HPLC-MS/MS.

    Science.gov (United States)

    Brandão, Pedro Francisco; Ramos, Rui Miguel; Almeida, Paulo Joaquim; Rodrigues, José António

    2017-02-08

    A new approach is proposed for the extraction and determination of carbonyl compounds in solid samples, such as wood or cork materials. Cork products are used as building materials due to their singular characteristics; however, little is known about its aldehyde emission potential and content. Sample preparation was done by using a gas-diffusion microextraction (GDME) device for the direct extraction of volatile aldehydes and derivatization with 2,4-dinitrophenylhydrazine. Analytical determination of the extracts was done by HPLC-UV, with detection at 360 nm. The developed methodology proved to be a reliable tool for aldehyde determination in cork agglomerate samples with suitable method features. Mass spectrometry studies were performed for each sample, which enabled the identification, in the extracts, of the derivatization products of a total of 13 aldehydes (formaldehyde, acetaldehyde, furfural, propanal, 5-methylfurfural, butanal, benzaldehyde, pentanal, hexanal, trans-2-heptenal, heptanal, octanal, and trans-2-nonenal) and 4 ketones (3-hydroxy-2-butanone, acetone, cyclohexanone, and acetophenone). This new analytical methodology simultaneously proved to be consistent for the identification and determination of aldehydes in cork agglomerates and a very simple and straightforward procedure.

  6. HPLC-Analysis of Polyphenolic Compounds in Gardenia jasminoides and Determination of Antioxidant Activity by Using Free Radical Scavenging Assays

    Directory of Open Access Journals (Sweden)

    Riaz Uddin

    2014-05-01

    Full Text Available Purpose: Gardenia jasminoides is a traditional medicinal plant rich in anti-inflammatory flavonoids and phenolic compounds and used for the treatment of inflammatory diseases and pain. In this present study, antioxidant potential of Gardenia jasminoides leaves extract was evaluated by using various antioxidant assays. Methods: Various antioxidant assays such as 1, 1-diphenyl-2-picrylhydrazyl (DPPH radical scavenging assay, reducing power and total antioxidant capacity expressed as equivalent to ascorbic acid were employed. Moreover, phenolic compounds were detected by high-performance liquid chromatography (HPLC coupled with diode-array detection. Results: The methanol extract showed significant free radical scavenging activities in DPPH radical scavenging antioxidant assays compared to the reference antioxidant ascorbic acid. Total antioxidant activity was increased in a dose dependent manner. The extract also showed strong reducing power. The total phenolic content was determined as 190.97 mg/g of gallic acid equivalent. HPLC coupled with diode-array detection was used to identify and quantify the phenolic compounds in the extracts. Gallic acid, (+-catechin, rutin hydrate and quercetin have been identified in the plant extracts. Among the phenolic compounds, catechin and rutin hydrate are present predominantly in the extract. The accuracy and precision of the presented method were corroborated by low intra- and inter-day variations in quantitative results in leaves extract. Conclusion: These results suggest that phenolic compounds and flavonoids might contribute to high antioxidant activities of Gardenia jasminoides leaves.

  7. Chapter 3. Determination of semivolatile organic compounds and polycyclic aromatic hydrocarbons in solids by gas chromatography/mass spectrometry

    Science.gov (United States)

    Zaugg, Steven D.; Burkhardt, Mark R.; Burbank, Teresa L.; Olson, Mary C.; Iverson, Jana L.; Schroeder, Michael P.

    2006-01-01

    A method for the determination of 38 polycyclic aromatic hydrocarbons (PAHs) and semivolatile organic compounds in solid samples is described. Samples are extracted using a pressurized solvent extraction system. The compounds of interest are extracted from the solid sample twice at 13,800 kilopascals; first at 120 degrees Celsius using a water/isopropyl alcohol mixture (50:50, volume-to-volume ratio), and then the sample is extracted at 200 degrees Celsius using a water/isopropyl alcohol mixture (80:20, volume-to-volume ratio). The compounds are isolated using disposable solid-phase extraction (SPE) cartridges containing divinylbenzene-vinylpyrrolidone copolymer resin. The cartridges are dried with nitrogen gas, and then sorbed compounds are eluted from the SPE material using a dichloromethane/diethyl ether mixture (80:20, volume-to-volume ratio) and passed through a sodium sulfate/Florisil SPE cartridge to remove residual water and to further clean up the extract. The concentrated extract is solvent exchanged into ethyl acetate and the solvent volume reduced to 0.5 milliliter. Internal standard compounds are added prior to analysis by capillary-column gas chromatography/mass spectrometry. Comparisons of PAH data for 28 sediment samples extracted by Soxhlet and the accelerated solvent extraction (ASE) method described in this report produced similar results. Extraction of PAH compounds from standard reference material using this method also compared favorably with Soxhlet extraction. The recoveries of PAHs less than molecular weight 202 (pyrene or fluoranthene) are higher by up to 20 percent using this ASE method, whereas the recoveries of PAHs greater than or equal to molecular weight 202 are equivalent. This ASE method of sample extraction of solids has advantages over conventional Soxhlet extraction by increasing automation of the extraction process, reducing extraction time, and using less solvent. Extract cleanup also is greatly simplified because SPE replaces

  8. Potential of LC Coupled to Fluorescence Detection in Food Metabolomics: Determination of Phenolic Compounds in Virgin Olive Oil

    Directory of Open Access Journals (Sweden)

    Romina P. Monasterio

    2016-09-01

    Full Text Available A powerful chromatographic method coupled to a fluorescence detector was developed to determine the phenolic compounds present in virgin olive oil (VOO, with the aim to propose an appropriate alternative to liquid chromatography-mass spectrometry. An excitation wavelength of 285 nm was selected and four different emission wavelengths (316, 328, 350 and 450 nm were simultaneously recorded, working therefore on “multi-emission” detection mode. With the use of commercially available standards and other standards obtained by semipreparative high performance liquid chromatography, it was possible to identify simple phenols, lignans, several complex phenols, and other phenolic compounds present in the matrix under study. A total of 26 phenolic compounds belonging to different chemical families were identified (23 of them were susceptible of being quantified. The proposed methodology provided detection and quantification limits within the ranges of 0.004–7.143 μg·mL−1 and 0.013–23.810 μg·mL−1, respectively. As far as the repeatability is concerned, the relative standard deviation values were below 0.43% for retention time, and 9.05% for peak area. The developed methodology was applied for the determination of phenolic compounds in ten VOOs, both monovarietals and blends. Secoiridoids were the most abundant fraction in all the samples, followed by simple phenolic alcohols, lignans, flavonoids, and phenolic acids (being the abundance order of the latter chemical classes logically depending on the variety and origin of the VOOs.

  9. Determination of total phenolic compound contents and antioxidant capacity of persimmon skin

    Directory of Open Access Journals (Sweden)

    M Mohamadi

    2012-05-01

    Full Text Available Due to the adverse side effects of synthetic antioxidants, the search for natural and safe antioxidants has become crucial. In this study, the total phenolic compound contents and antioxidants activity of persimmon skin was investigated. The extraction was carried out by means of maceration method using ethanol and methanol solvents with ratio of 1 part persimmon skin to 5 parts of solvents. Afterwards, the total phenolic compounds and antioxidants activity was measured. According to the results, ethanolic and methanolic extracts contained 255.6 and 214.15 mg gallic acid per 100 g of persimmon skin, respectively. Moreover, ethanolic extracts showed a higher activity for scavenging free radicals compared to methanolic extracts.

  10. Determination of nitrosourea compounds in brain tissue by gas chromatography and electron capture detection.

    Science.gov (United States)

    Hassenbusch, S J; Colvin, O M; Anderson, J H

    1995-07-01

    A relatively simple, high-sensitivity gas chromatographic assay is described for nitrosourea compounds, such as BCNU [1,3-bis(2-chloroethyl)-1-nitrosourea] and MeCCNU [1-(2-chloroethyl)-3-(trans-4-methylcyclohexyl)-1-nitrosourea], in small biopsy samples of brain and other tissues. After extraction with ethyl acetate, secondary amines in BCNU and MeCCNU are derivatized with trifluoroacetic anhydride. Compounds are separated and quantitated by gas chromatography using a capillary column with temperature programming and an electron capture detector. Standard curves of BCNU indicate a coefficient of variance of 0.066 +/- 0.018, a correlation coefficient of 0.929, and an extraction efficiency from whole brain of 68% with a minimum detectable amount of 20 ng in 5-10 mg samples. The assay has been facile and sensitive in over 1000 brain biopsy specimens after intravenous and intraarterial infusions of BCNU.

  11. Determination of the Temperature Dependence of Heat Capacity for Some Molecular Crystals of Nitro Compounds

    Science.gov (United States)

    Kovalev, Yu. M.; Kuropatenko, V. F.

    2018-05-01

    An analysis of the existing approximations used for describing the dependence of heat capacity at a constant volume on the temperature of a molecular crystal has been carried out. It is shown that the considered Debye and Einstein approximations do not enable one to adequately describe the dependence of heat capacity at a constant volume on the temperature of the molecular crystals of nitro compounds. This inference requires the development of special approximations that would describe both low-frequency and high-frequency parts of the vibrational spectra of molecular crystals. This work presents a universal dependence allowing one to describe the dependence of heat capacity at a constant volume on temperature for a number of molecular crystals of nitro compounds.

  12. Determination of non-volatile radiolytic compounds in ethylene co-vinyl alcohol

    International Nuclear Information System (INIS)

    Kothapalli, A.; Sadler, G.

    2003-01-01

    The use of ionizing radiation on food contact polymers is increasing due to the critical role of the package in holding or containing the irradiated foods [Food Add. Contam. 18(6) (2001) 475]. Irradiation benefits the food if properly applied and the food is pre-packaged prior to irradiation to protect it from subsequent recontamination. The United States Food and Drug Administration (USFDA) has approved the use of ionizing radiation within the dosage range of 0-60 kGy on limited films since the 1960s [USFDA 21CFR 179.45]. The obstacle in the way of approval of additional polymers is that FDA fears that these materials may undergo changes during irradiation producing toxic radiolytic fragments. Ethylene co-vinyl alcohol (EVOH), which is often used in food applications, is not approved by the FDA for pre-packaged irradiated foods. The present work examines the non-volatile radiolytic compounds, which may be formed due to exposure to gamma irradiation at the dosage levels of 3 and 10 kGy versus a non-radiated control. Irradiated EVOH is subjected to extraction with 95:5 ethanol and water (by volume) as the food simulating solvent (FSS) for a period of 10 days at 40 deg. C, which models the amount of radiolytic compound a food would extract in 1 year [USFDA Chemistry Requirement for Food Contact Notification]. The FSS is then analyzed for the presence of non-volatile compounds using advanced liquid chromatographic techniques. The chromatograms obtained from different dosages show that non-volatile radiolytic compounds are not formed in EVOH and it would, therefore be in compliance with safety demands of USFDA [Available at: http://www.cfsan.fda.gov/~dms/opa-guid.htmlref and http://www.access.gpo.gov/nara/cfr/cfr-table-search.htmlpage1

  13. Determination of Carbonyl Compounds in Cigarette Mainstream Smoke. The CORESTA 2010 Collaborative Study and Recommended Method

    Directory of Open Access Journals (Sweden)

    Intorp M

    2014-12-01

    Full Text Available A recommended method has been developed and published by CORESTA, applicable to the quantification of selected carbonyl compounds (acetaldehyde, formaldehyde, acetone, acrolein, methyl ethyl ketone, crotonaldehyde, propionaldehyde and butyraldehyde in cigarette mainstream smoke. The method involved smoke collection in impinger traps, derivatisation of carbonyls with 2,4-dinitrophenylhydrazine (DNPH, separation of carbonyl hydrazones by reversed phase high performance liquid chromatography and detection by ultra violet or diode array.

  14. Determination of non-volatile radiolytic compounds in ethylene co-vinyl alcohol

    Science.gov (United States)

    Kothapalli, A.; Sadler, G.

    2003-08-01

    The use of ionizing radiation on food contact polymers is increasing due to the critical role of the package in holding or containing the irradiated foods [Food Add. Contam. 18(6) (2001) 475]. Irradiation benefits the food if properly applied and the food is pre-packaged prior to irradiation to protect it from subsequent recontamination. The United States Food and Drug Administration (USFDA) has approved the use of ionizing radiation within the dosage range of 0-60 kGy on limited films since the 1960s [USFDA 21CFR 179.45]. The obstacle in the way of approval of additional polymers is that FDA fears that these materials may undergo changes during irradiation producing toxic radiolytic fragments. Ethylene co-vinyl alcohol (EVOH), which is often used in food applications, is not approved by the FDA for pre-packaged irradiated foods. The present work examines the non-volatile radiolytic compounds, which may be formed due to exposure to gamma irradiation at the dosage levels of 3 and 10 kGy versus a non-radiated control. Irradiated EVOH is subjected to extraction with 95:5 ethanol and water (by volume) as the food simulating solvent (FSS) for a period of 10 days at 40 °C, which models the amount of radiolytic compound a food would extract in 1 year [USFDA Chemistry Requirement for Food Contact Notification]. The FSS is then analyzed for the presence of non-volatile compounds using advanced liquid chromatographic techniques. The chromatograms obtained from different dosages show that non-volatile radiolytic compounds are not formed in EVOH and it would, therefore be in compliance with safety demands of USFDA [Available at: http://www.cfsan.fda.gov/~dms/opa-guid.html#ref and http://www.access.gpo.gov/nara/cfr/cfr-table-search.html#page1].

  15. Wet effluent diffusion denuder technique and the determination of volatile organic compounds in air. II. Monoterpenes

    Czech Academy of Sciences Publication Activity Database

    Sklenská, Jana; Broškovičová, Anna; Večeřa, Zbyněk

    2002-01-01

    Roč. 973, 1-2 (2002), s. 211-216 ISSN 0021-9673 R&D Projects: GA ČR GA203/98/0943 Grant - others:SPSDII(XE) EV/02/11 Institutional research plan: CEZ:AV0Z4031919 Keywords : wet effluent denuder technique * volatile organic compounds * monoterpenes Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.098, year: 2002

  16. Determination of Fluorine in Fluoro-Organic Compounds in Low Concentrations in Air

    Science.gov (United States)

    1944-06-27

    Analysis of 2-Fluoroethanol in Air ..... SUMMARY BIBLIOGRAPHY 15 APPENDIX , 16 FIGURE 1 Apparatus PLATE 1 CDS Scrubber SECRET ) SECRET...liter, and 68$ at 1 - 2 mg. per liter. By using two scrubbers in series, 90$ of di-isopropyl fluorophosphate was recovered at a concentration of 1 to 2...chromic acid and detection of HP by etching of the glass container ; (5) scrub- bing the gas with ammonia and decomposing the fluoro-organic compound4

  17. Determination of the ultrasound power effects on flavonoid compounds from Psidium guajava L. using ANFIS

    Science.gov (United States)

    Ratu Ayu, Humairoh; Suryono, Suryono; Endro Suseno, Jatmiko; Kurniawati, Ratna

    2018-05-01

    The Adaptive Neural Fuzzy Inference System (ANFIS) model was used to predict and optimize the content of flavonoid compounds in guava leaves (Psidium Guajava L.). The extraction process was carried out by using ultrasound assisted extraction (UAE) with the variable parameters: temperature ranging from 25°C to 35°C, ultrasonic frequency (30 - 40 kHz) and extraction time (20 - 40 minutes). ANFIS learning procedure began by providing the input variable data set (temperature, frequency and time) and the output of the flavonoid compounds from the experiments that had been done. Subtractive clustering methods was used in the manufacture of FIS (fuzzy inference system) structures by varying the range of influence parameters to generate the ANFIS system. The ANFIS trainingsconducted wereaimed at minimum error value. The results showed that the best ANFIS models used a subtractive clustering method, in which the ranges of influence 0.1 were 0.70 x 10-4 for training RMSE, 8.11 for testing RMSE, 2.7 % MAPE, and 7.72 MAE. The optimum condition was obtained at a temperature of 35°C and frequency of 40 kHz, for 30 minutes. This result proves that the ANFIS model can be used to predict the content of flavonoid compounds in guava leaves.

  18. Determination of drugs and drug-like compounds in different samples with direct analysis in real time mass spectrometry.

    Science.gov (United States)

    Chernetsova, Elena S; Morlock, Gertrud E

    2011-01-01

    Direct analysis in real time (DART), a relatively new ionization source for mass spectrometry, ionizes small-molecule components from different kinds of samples without any sample preparation and chromatographic separation. The current paper reviews the published data available on the determination of drugs and drug-like compounds in different matrices with DART-MS, including identification and quantitation issues. Parameters that affect ionization efficiency and mass spectra composition are also discussed. Copyright © 2011 Wiley Periodicals, Inc.

  19. An approach to determination of phenolic compounds in seawater using SPME-GC-MS based on SWCNTs coating

    Science.gov (United States)

    Zhu, Jia; Wang, Ying; Zeng, Lin

    2016-08-01

    Phenolic compounds have become one kind of the important pollutants of the marine environment. Single-walled Carbon nanotubes, as one-dimensional nano materials, have light weight and perfect hexagonal structure of connections, with many unusual mechanical, chemical and electrical properties. In recent years, with the research of carbon nanotubes and other nano materials, the application prospect is also constantly discussed. In this paper, homemade single-walled carbon nanotubes (SWCNTs) coating was used for establishing an analytical approach to the determination of five kinds of phenolic compounds in seawater using SPME-GC-MS. Optimal conditions: After saturation was conducted with NaCl, and pH was adjusted to 2.0 with H2SO4, the extract was immersed in a water bath at 40°C for GC-MS determination through 40-min agitating extraction at 500 rmin-1 and 3-min desorption at 280°C. The liniearities ranged between 0.01-100 μg L-1, and the determination limits ranged between 1.5-10 ng L-1. The relative standard deviation (RSD, n = 5) was less than 6.5%. For the phenolic compounds obtained from the spiked recovery test for actual seawater samples, the rates of recovery were 87.5%-101.7%, and the RSDs were less than 8.8%, which met the requirements of determination. Due to its simplicity, high efficiency and low consumption, this approach is suitable for the analysis of trace amounts of phenolic compounds in marine waters.

  20. Application of the crystalline structure determination method by X-ray diffraction to natural products and organic compounds

    International Nuclear Information System (INIS)

    Vencato, I.

    1984-01-01

    The structures of two natural compounds, a synthetic phosphate and a copper complexe were determined and the structure of another copper complex was refined. The reflection intensities were measured with a CAD-4 automatic diffractometer. The structures were solved by direct methods using either MULTAN-80 or the Patterson function and were refined by the least squares method, with a full matrix. (E.G.) [pt

  1. Structural determination of some uranyl compounds by vibrational spectroscopy; Determinacion estructural de algunos compuestos de uranilo por espectroscopia vibracional

    Energy Technology Data Exchange (ETDEWEB)

    Rodriguez S, A.; Martinez Q, E

    1990-07-15

    The vibrational spectra of different uranyl compounds has been studied and of it spectral information has been used the fundamental asymmetric vibrational frequency, to determine the length and constant bond force U=O by means of the combination of the concept of absorbed energy and the mathematical expression of Badger modified by Jones. It is intended a factor that simplifies the mathematical treatment and the results are compared with the values obtained for other methods. (Author)

  2. Development of the extraction method for the simultaneous determination of butyl-, phenyl- and octyltin compounds in sewage sludge.

    Science.gov (United States)

    Zuliani, Tea; Lespes, Gaetane; Milacic, Radmila; Scancar, Janez

    2010-03-15

    The toxicity and bioaccumulation of organotin compounds (OTCs) led to the development of sensitive and selective analytical methods for their determination. In the past much attention was assigned to the study of OTCs in biological samples, water and sediments, coming mostly from marine environment. Little information about OTCs pollution of terrestrial ecosystems is available. In order to optimise the extraction method for simultaneous determination of butyl-, phenyl- and octyltin compounds in sewage sludge five different extractants (tetramethylammonium hydroxide, HCl in methanol, glacial acetic acid, mixture of acetic acid and methanol (3:1), and mixture of acetic acid, methanol and water (1:1:1)), the presence or not of a complexing agent (tropolone), and the use of different modes of extraction (mechanical stirring, microwave and ultrasonic assisted extraction) were tested. Extracted OTCs were derivatised with sodium tetraethylborate and determined by gas chromatography coupled with mass spectrometer. Quantitative extraction of butyl-, phenyl- and octyltin compounds was obtained by the use of glacial acetic acid as extractant and mechanical stirring for 16h or sonication for 30 min. The limits of detection and quantification for OTCs investigated in sewage sludge were in the ng S ng(-1) range. Copyright (c) 2009 Elsevier B.V. All rights reserved.

  3. VOLATILE COMPOUNDS OF LITHRAEA CAUSTICA (LITRE) DETERMINATED BY SOLID PHASE MICRO-EXTRACTION (SPME)

    OpenAIRE

    GARBARINO, JUAN A; SALVATORE, GIUSEPPE; PIVANOVO, MARISA; CHAMY, MARÍA CRISTINA; NICOLETTI, MARCELLO; DE IOANNES, ALFREDO

    2002-01-01

    The head space of the aerial parts of Lithraea caustica was analyzed by Solid Phase Micro-Extraction (SPME) technique, obtaining as main volatile compounds the monoterpenes, myrcene, a -pinene, , p-cymene and limonene, as well as the sesquiterpene caryophylene. De las partes áereas de Lithraea caustica y usando la técnica de Micro-Extracción en Fase Sólida (MEFS), fueron identificados y cuantificados los principales compuestos volátiles: los monoterpenos, mirceno, a -pineno, p-cimeno y lim...

  4. Spectrographic determination of lanthanides in high-purity uranium compounds, after chromatographic separation by alumina-hydrofluoric acid

    International Nuclear Information System (INIS)

    Lordello, A.R.; Abrao, A.

    1979-01-01

    A method is presented for the determination of fourteen rare earth elements in high-purity uranium compounds by emission spectrography. The rare earths are chromatographically separated from uranium by using alumina-hydrofluoric acid. Lanthanum is used both as collector and internal standard. The technique of excitation involves a total consumption of the sample in a 17 ampere direct current arc. The range of determination is about 0.005 to 0.5 μg/g uranium. The coefficient of variation for Pr, Ho, Dy, Er, Tm, Lu, Gd and Tb amounts to 10%. (Author) [pt

  5. Work Tasks as Determinants of Grain Dust and Microbial Exposure in the Norwegian Grain and Compound Feed Industry.

    Science.gov (United States)

    Straumfors, Anne; Heldal, Kari Kulvik; Wouters, Inge M; Eduard, Wijnand

    2015-07-01

    The grain and compound feed industry entails inevitable risks of exposure to grain dust and its microbial content. The objective of this study was therefore to investigate task-dependent exposure differences in order to create knowledge basis for awareness and exposure reducing measures in the Norwegian grain and compound feed industry. A total of 166 samples of airborne dust were collected by full-shift personal sampling during work in 20 grain elevators and compound feed mills during one autumn season and two winter seasons. The personal exposure to grain dust, endotoxins, β-1→3-glucans, bacteria, and fungal spores was quantified and used as individual outcomes in mixed models with worker nested in company as random effect and different departments and tasks as fixed effects. The exposure levels were highest in grain elevator departments. Exposure to endotoxins was particularly high. Tasks that represented the highest and lowest exposures varied depending on the bioaerosol component. The most important determinants for elevated dust exposure were cleaning and process controlling. Cleaning increased the dust exposure level by a factor of 2.44 of the reference, from 0.65 to 1.58mg m(-3), whereas process controlling increased the dust exposure level by a factor of 2.97, from 0.65 to 1.93mg m(-3). Process controlling was associated with significantly less grain dust exposure in compound feed mills and the combined grain elevators and compound feed mills, than in grain elevators. The exposure was reduced by a factor of 0.18 and 0.22, from 1.93 to 0.34mg m(-3) and to 0.42mg m(-3), respectively, compared with the grain elevators. Inspection/maintenance, cleaning, and grain rotation and emptying were determinants of higher exposure to both endotoxin and β-1→3-glucans. Seed winnowing was in addition a strong determinant for endotoxin, whereas mixing of animal feed implied higher β-1→3-glucan exposure. Cleaning was the only task that contributed significantly to

  6. Leaf enclosure measurement for determining marijuana volatile organic compound emission factors

    Science.gov (United States)

    Wang, C. T.; Vizuete, W.; Wiedinmyer, C.; Ashworth, K.; Harley, P. C.; Ortega, J. V.

    2017-12-01

    In 2014, Colorado became the first US state to legalize the industrial-scale cultivation of marijuana plants. There are now more than 700 marijuana cultivation facilities (MCFs) in operation in the greater Denver area. High concentrations of biogenic volatile organic compounds (VOCs), predominantly monoterpenes (C10H16) such as alpha-pinene, myrcene, and limonene have been observed in the grow rooms of MCFs, suggesting MCFs have the potential to release a significant amount of reactive VOCs into the atmosphere. Further, many MCFs are located in the urban core, where other urban emission sources are concentrated, resulting in interactions which can lead to the formation of ozone, impacting air quality. The little research done on marijuana has focused on indoor air quality and occupational exposure, or identification of the compounds associated with the characteristic smells of marijuana plants. We know of no previous studies that have identified or quantified the monoterpene emission rates from marijuana. Here, we collected air samples from leaf enclosures from different marijuana clones at different growth stages onto sorbent cartridges. These samples were analyzed using GC-MS/-FID to identify and quantify the VOCs emitted by growing marijuana plants. These results were then used to estimate basal emission rates at standard conditions (T=30 C, PPFD = 1000 umol/m2/s) using standard algorithms. We discuss the potential impact on air quality from these VOCs emitted into the atmosphere using air quality models.

  7. Determination of volatile organic compounds pollution sources in malaysian drinking water using multivariate analysis.

    Science.gov (United States)

    Soh, Shiau-Chian; Abdullah, Md Pauzi

    2007-01-01

    A field investigation was conducted at all water treatment plants throughout 11 states and Federal Territory in Peninsular Malaysia. The sampling points in this study include treatment plant operation, service reservoir outlet and auxiliary outlet point at the water pipelines. Analysis was performed by solid phase micro-extraction technique with a 100 microm polydimethylsiloxane fibre using gas chromatography with mass spectrometry detection to analyse 54 volatile organic compounds (VOCs) of different chemical families in drinking water. The concentration of VOCs ranged from undetectable to 230.2 microg/l. Among all of the VOCs species, chloroform has the highest concentration and was detected in all drinking water samples. Average concentrations of total trihalomethanes (THMs) were almost similar among all states which were in the range of 28.4--33.0 microg/l. Apart from THMs, other abundant compounds detected were cis and trans-1,2-dichloroethylene, trichloroethylene, 1,2-dibromoethane, benzene, toluene, ethylbenzene, chlorobenzene, 1,4-dichlorobenzene and 1,2-dichloro - benzene. Principal component analysis (PCA) with the aid of varimax rotation, and parallel factor analysis (PARAFAC) method were used to statistically verify the correlation between VOCs and the source of pollution. The multivariate analysis pointed out that the maintenance of auxiliary pipelines in the distribution systems is vital as it can become significant point source pollution to Malaysian drinking water.

  8. German standard methods for the examination of water, waste water and sludge: Anions (group D), determination of phosphorus compounds (D 11)

    International Nuclear Information System (INIS)

    1982-01-01

    The following method for the determination of phosphorus compounds in water and waste water is proposed. In acid solutions phosphate ions form with molybdate and antimony ions an antimonylphosphorusmolybdate-complex which is reduced to phosphorusmolybdenumblue by ascorbic acid. The intensity of the colour is determined by photometric methods. Polyphosphates and some organic phosphorus compounds are hydrolysed to orthophosphate by cooking in strong acid solutions. Other stable phosphorus compounds are decomposed by strong oxidizing agents (potassiumperoxidisulfate or nitric acid). (VG) [de

  9. Comparison of GC/MSD and GC/AED for the determination of organotin compounds in the environment

    Energy Technology Data Exchange (ETDEWEB)

    Staeb, J.A. (Inst. of Environmental Studies, Free Univ., Amsterdam (Netherlands)); Cofino, W.P. (Inst. of Environmental Studies, Free Univ., Amsterdam (Netherlands)); Hattum, B. van (Inst. of Environmental Studies, Free Univ., Amsterdam (Netherlands)); Brinkman, U.A.T. (Dept. of Analytical Chemistry, Free Univ., Amsterdam (Netherlands))

    Methods are described for the analysis of environmental samples like water, sediment and suspended matter for the determination of all organotin compounds (OTs) that are currently used as biocides: Tributyltin (TBT) triphenyltin (TPT), tricyclohexyltin (TCT) and fenbutatin oxide (FBTO). In water also five degradation products (di and mono substituted analogs) can be determined. Alkylation using a Grignard reagent was used to obtain OT derivatives amenable to gas chromatography (GC). Both methylation and pentylation have been employed for derivatization prior to GC analysis. The present results show that derivatization efficiencies for TPT, TCT and FBTO at trace levels are higher using methylation than pentylation. Detection limits for each type of sample matrix were determined using GC/Mass Selective Detection (GC/MSD) and GC/Atomic Emission Detection (AED). In sediment and suspended matter only tri-substituted OTs (i.e. the parent compounds) could be determined. Detection limits ranged from 0.2 to 10 ng/g dry weight. FBTO, not previously detected in environmental samples, was found at levels of 4 and 11 ng/g in a suspended matter sample and a sediment sample, respectively. In water the OTs and their degradation products were determined at levels of 1-10 ng/l (as tin) using 200 ml water samples. (orig.)

  10. Simultaneous determination of five active compounds in chimonanthus nitens by double-development HPTLC and scanning densitometry

    Directory of Open Access Journals (Sweden)

    Zhou Bin

    2012-05-01

    Full Text Available Abstract Background Chimonanthus nitens (family Calycanthaceae, Shanlamei in Chinese, is an unique species in China. The extract of dried leaves of Chimonanthus nitens has anti-inflammatory, antipyretic and antitussive effects. Terpenes, coumarins, and flavonoids are usually regarded as the main active components. Therefore, simultaneous determination of these compounds is very important to control the quality of Chimonanthus nitens. Results A double-development TLC method was developed for simultaneous analysis of five compounds in Chimonanthus nitens. The chromatography was performed on silica gel 60 plate with chloroform-methanol (9∶1, v/v and petroleum ether-ethyl acetate (10∶1, v/v as mobile phase for twice development. Their characteristic TLC profiles were observed under UV light at 365 nm and the bands were then revealed by reaction with 1% vanillin-H2SO4 solution. Quantification of three monoterpenes was achieved by densitometry at 545 nm (β-caryophyllene or 606 nm (cineole and linalool. Two coumarins (scopoletin and scoparone were determined by densitometry at 340 nm with filter wavelength of 370 nm. The investigated compounds had good linearity (R2 >0.99 within test ranges. Conclusions The developed double-development TLC method is helpful to control the quality of Chimonanthus nitens, which is simple and accurate.

  11. Determination of volatile organic compounds from biowaste and co-fermentation biogas plants by single-sorbent adsorption.

    Science.gov (United States)

    Salazar Gómez, J I; Lohmann, H; Krassowski, J

    2016-06-01

    Characterisation of biogases is normally dedicated to the online monitoring of the major components methane and carbon dioxide and, to a lesser extent, to the determination of ammonia and hydrogen sulphide. For the case of Volatile Organic Compounds (VOCs), much less attention is usually paid, since such compounds are normally removed during gas conditioning and with exception of sulphur compounds and siloxanes represent a rather low risk to conventional downstream devices but could be a hindrance for fuel cells. However, there is very little information in the literature about the type of substances found in biogases generated from biowaste or co-fermentation plants and their concentration fluctuations. The main aim of this study was to provide information about the time dependencies of the VOCs in three biogas plants spread out through Germany from autumn until summer, which have different process control, in order to assess their potential as biofuels. Additionally, this study was an attempt to establish a correlation between the nature of the substrates used in the biogas plants and the composition of the VOCs present in the gas phase. Significant time-dependent variations in concentration were observed for most VOCs but only small changes in composition were observed. In general, terpenes and ketones appeared as the predominant VOCs in biogas. Although for substances such as esters, sulphur-organic compounds and siloxanes the average concentrations observed were rather low, they exhibited significant concentration peaks. The second biogas plant which operates with dry fermentation was found to contain the highest levels of VOCs. The amount of total volatile organic compounds (TVOCs) for the first, second and third biogas plants ranged from 35 to 259 mg Nm(-3), 291-1731 mg Nm(-3) and 84-528 mg Nm(-3), respectively. Copyright © 2016 Elsevier Ltd. All rights reserved.

  12. Use of electrothermal atomization for determining metallic impurities in nuclearly pure uranium compounds

    International Nuclear Information System (INIS)

    Franco, M.B.

    1986-01-01

    Atomic absorption spectrometry with electrothermal atomization was used for the determination of Al, Cd, Cr, Fe, Mn, Mo and Ni as impurities in uranium oxide samples. The determinations were performed in solubilized samples both with and without uranium separation as well as in solid samples. (Author) [pt

  13. Use of electrothermal atomization for determining metallic impurities in nuclearly pure uranium compounds

    International Nuclear Information System (INIS)

    Franco, M.B.

    1985-01-01

    Atomic absorption spectrometry with electrothermal atomization was used for the determination of Al, Cd, Cr, Fe, Mn, Mo and Ni as impurities in uranium oxide samples. The determinations were performed in solubilized samples both with and without uranium separation as well as in solid samples. (Author) [pt

  14. Determination of taste-active compounds of a bitter Camembert cheese by omission tests.

    Science.gov (United States)

    Engel, E; Septier, C; Leconte, N; Salles, C; Le Quere, J L

    2001-11-01

    The taste-active compounds of a Camembert cheese selected for its intense bitterness defect were investigated. The water-soluble fraction (WSE) was extracted with pure water and fractionated by successive tangential ultrafiltrations and nanofiltration. The physicochemical assessment of these fractions led to the construction of a model WSE which was compared by sensory evaluation to the crude water-soluble extract, using a panel of 16 trained tasters. As no significant difference was perceived, this model WSE was then used directly or mixed with other cheese components for omission tests. Among the main taste characteristics of the WSE (salty, sour, umami and bitter), bitterness was found to be due to small peptides whose mass distribution was obtained by RPHPLC-MS (400-3000 Da) and whose taste properties are discussed.

  15. Species analysis of organomercury compounds to determine their biopathways at contaminated sites

    International Nuclear Information System (INIS)

    Hintelmann, H.

    1993-01-01

    The environmental behavior of organomercury compounds with special regard to methyl-mercury(II) was investigated. Organomercury species were extraced with a solution of dithizone in chloroform whereas methylmercury(II) is also extractable using HCl/Toluol. A newly developed HPLC/AFS-system was used as the analytical method. The methylmercury(II) content in river Elbe sediments is controlled by the content of sulfidic sulfur. The crucial point for the formation of methylmercury(II) is the microbial activity in the sediments. Besides methylmercury(II) ethylmercury(II) was found in river Koesseine sediments (Marktredwitz). Microbial biofilms are capable of accumulating methylmercury(II) to a factor of 10 5 when compared to the culture solution. (orig.). 62 figs., 47 tabs [de

  16. Study of electrical transport properties of (U 1- xY x)RuP 2Si 2

    Science.gov (United States)

    Radha, S.; Park, J.-G.; Roy, S. B.; Coles, B. R.; Nigam, A. K.; McEwen, K. A.

    1996-02-01

    Electrical resistivity and magnetoresistance ( {δϱ}/{ϱ}) measurements on a series of (U 1- xY x)Ru 2Si 2 (0 ⩽ x ⩽ 0.9) compounds in the temperature range 4.2-300 K and in magnetic fields up to 45 kOe are reported. The resistivity measurements do not show any signature of antiferromagnetism for x > 0.5. The compound URu 2Si 2 exhibits a large, positive ( {δϱ}/{ϱ}) presumably due to destruction of Kondo coherence as well as due to antiferromagnetism. The presence of even 5% Y at U-site weakens the Kondo coherence and reduces the magnetoresistance considerably.

  17. Determination of ten perfluorinated compounds in bluegill sunfish (Lepomis macrochirus) fillets

    International Nuclear Information System (INIS)

    Delinsky, Amy D.; Strynar, Mark J.; Nakayama, Shoji F.; Varns, Jerry L.; Ye, XiBiao; McCann, Patricia J.; Lindstrom, Andrew B.

    2009-01-01

    A rigorous solid phase extraction/liquid chromatography/tandem mass spectrometry method for the measurement of 10 perfluorinated compounds (PFCs) in fish fillets is described and applied to fillets of bluegill sunfish (Lepomis macrochirus) collected from selected areas of Minnesota and North Carolina. The 4 PFC analytes routinely detected in bluegill fillets were perfluorooctane sulfonate (PFOS), perfluorodecanoic acid (C10), perfluoroundecanoic acid (C11), and perflurododecanoic acid (C12). Measures of method accuracy and precision for these compounds showed that calculated concentrations of PFCs in spiked samples differed by less than 20% from their theoretical values and that the %RSD for repeated measurements was less than 20%. Minnesota samples were collected from areas of the Mississippi River near historical PFC sources, from the St. Croix River as a background site, and from Lake Calhoun, which has no documented PFC sources. PFOS was the most prevalent PFC found in the Minnesota samples, with median concentrations of 47.0-102 ng/g at locations along the Mississippi River, 2.08 ng/g in the St. Croix River, and 275 ng/g in Lake Calhoun. North Carolina samples were collected from two rivers with no known historical PFC sources. PFOS was the predominant analyte in fish taken from the Haw and Deep Rivers, with median concentrations of 30.3 and 62.2 ng/g, respectively. Concentrations of C10, C11, and C12 in NC samples were among the highest reported in the literature, with respective median values of 9.08, 23.9, and 6.60 ng/g in fish from the Haw River and 2.90, 9.15, and 3.46 ng/g in fish from the Deep River. These results suggest that PFC contamination in freshwater fish may not be limited to areas with known historical PFC inputs.

  18. Optical contrast spectra studies for determining thickness of stage-1 graphene-FeCl{sub 3} intercalation compounds

    Energy Technology Data Exchange (ETDEWEB)

    Han, Wen-Peng, E-mail: han-wenpeng@163.com, E-mail: yunze.long@163.com; Yan, Xu; Zhao, Hui [College of Physics, Qingdao University, Qingdao 266071 (China); Li, Qiao-Qiao; Lu, Yan [State Key Laboratory for Superlattices and Microstructures, Institute of Semiconductors, Chinese Academy of Sciences, Beijing 100083 (China); Long, Yun-Ze, E-mail: han-wenpeng@163.com, E-mail: yunze.long@163.com [College of Physics, Qingdao University, Qingdao 266071 (China); Collaborative Innovation Center for Low-Dimensional Nanomaterials and Optoelectronic Devices, Qingdao University, Qingdao 266071 (China)

    2016-07-15

    Because of novel features in their structural, electronic, magnetic and optical properties, especially potential applications in nanoelectronics, the few-layer graphene intercalation compounds (FLGICs) have been intensively studied recently. In this work, the dielectric constant of the doped graphene of stage-1 FeCl{sub 3}-GIC is obtained by fitting the optical contrast spectra. And fully intercalated stage-1 FeCl{sub 3}-FLGICs were prepared by micromechanical cleavage method from graphite intercalation compounds (GICs) for the first time. Finally, we demonstrated that the thickness of stage-1 FeCl{sub 3}-GICs by micromechanical cleavage can be determined by optical contrast spectra. This method also can be used to other FLGICs, such as SbCl{sub 5}-FLGICs and AuCl{sub 5}-FLGICs, etc.

  19. Determination of the solubility of low volatility liquid organic compounds in water using volatile-tracer assisted headspace gas chromatography.

    Science.gov (United States)

    Zhang, Shu-Xin; Chai, Xin-Sheng; Barnes, Donald G

    2016-02-26

    This study reports a new headspace gas chromatographic method (HS-GC) for the determination of water solubility of low volatility liquid organic compounds (LVLOs). The HS-GC analysis was performed on a set of aqueous solutions containing a range of concentrations of toluene-spiked (as a tracer) LVLOs, from under-saturation to over-saturation. A plot of the toluene tracer GC signal vs. the concentration of the LVLO results in two lines of different slopes that intersect at the concentration corresponding to the compound's solubility in water. The results showed that the HS-GC method has good precision (RSD waters of environmental and biological systems. Copyright © 2016 Elsevier B.V. All rights reserved.

  20. [Fast determination of contents of nutrients and stone powder in compound fertilizer using near infrared diffuse reflectance spectroscopy].

    Science.gov (United States)

    Guo, Zheng; Yuan, Hong-Fu; Zhang, Xian; Song, Chun-Feng; Li, Xiao-Yu; Xie, Jin-Chun

    2011-06-01

    In the present paper, a new approach to fast determination of contents of nutrients, including total nitrogen content (N), P2O5 content (P) and K2O content (K), and of stone powder content in compound fertilizer composed of urea, ammonium dihydrogen phosphate, potassium chloride and stone powder was proposed using near infrared diffuse reflectance spectroscopy. PLS models of N, P and stone powder content were built with the SEP values of 0.8, 0.8 and 1.4 respectively. The information on which stone powder content model was built is the spectrum of crystal water existing in stone powder. K content was calculated using other ingredientcontents by normalization principle with a SEP value of 1.5. Although the SEP values are a little larger than the reproducibility errors of the GB/T methods which are conventional methods, the new method can be accepted by situ quality control in the production process of compound fertilizer.

  1. Standard test method for determination of impurities in nuclear grade uranium compounds by inductively coupled plasma mass spectrometry

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2010-01-01

    1.1 This test method covers the determination of 67 elements in uranium dioxide samples and nuclear grade uranium compounds and solutions without matrix separation by inductively coupled plasma mass spectrometry (ICP-MS). The elements are listed in Table 1. These elements can also be determined in uranyl nitrate hexahydrate (UNH), uranium hexafluoride (UF6), triuranium octoxide (U3O8) and uranium trioxide (UO3) if these compounds are treated and converted to the same uranium concentration solution. 1.2 The elements boron, sodium, silicon, phosphorus, potassium, calcium and iron can be determined using different techniques. The analyst's instrumentation will determine which procedure is chosen for the analysis. 1.3 The test method for technetium-99 is given in Annex A1. 1.4 The values stated in SI units are to be regarded as standard. 1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish ...

  2. Determination of aminoglycoside antibiotics using complex compounds of chromotropic acid bisazoderivatives with rare earth ions

    International Nuclear Information System (INIS)

    Alykov, N.M.

    1981-01-01

    Studies of complex formation of bisazo derivatives of chromotropic acid with rare earth ions and aminoglycoside antibiotics have made it possible to choose carboxyarsenazo, orthanyl R and carboxynitrazo as highly sensitive reagents for determining aminoglycoside antibiotics. Conditions have been found for the formation of precipitates of different-ligand complexes containing rare earth ions, bisazo derivatives of chromotropic acid and aminogylcoside antibiotics. A procedure has been worked out of determining the antibiotics in biological samples with carboxyarsenazo [ru

  3. Determination of the migration of a plasticizer by 14C-labelled compounds

    International Nuclear Information System (INIS)

    Troparevsky, Alejandro; Pisarello de Troparevsky, M.L.; Mitta, A.E.A.

    1975-05-01

    The migration rate of a plasticizer (dioctyl phthlate 14 C) from a P.V.C. film, with different media in contact with it, was determined by measurements of radioactivity in the extraction liquids. Mineral oil, vegetal, oil aliphatic hidrocarbon and detergent solution were used for this purpose. The resulting figures were compared to those obtained from weight loss determinations and in some cases the percentage of ''swelling'' of the plastic could be established. (author)

  4. Sample preservation for determination of organic compounds: microwave versus freeze-drying

    International Nuclear Information System (INIS)

    Popp, M.; Lied, W.; Meyer, A.J.; Richter, A.; Schiller, P.; Schwitte, H.

    1996-01-01

    In search of a reliable drying method, which might be used even under field conditions, microwave drying was compared to freeze-drying of plant material. Leaves of Ananas comosus and Avicennia germinans as well as buds and phloem of Acer pseudoplatanus were used and checked for one or more of the following substances: sugars, sugar alcohols, organic and amino acids, total nitrogen, and glycinebetaine. With most samples good agreement was achieved between the two drying methods. Only in the case of the Ananas comosus leaves, which exhibited low pH and high water content, did appreciable differences occur in organic and amino acids. Besides that, sucrose was the compound most susceptible to alterations, which was especially evident when leaves of Sambucus nigra were dried in the two different compartments (condenser compartment, drying bell jar) of the freeze-dryer in use. For Ananas comosus leaf samples it was shown that microwaving can also be used prior to extraction of tissue sap. (author)

  5. Radiometric analyzer for boron content determination in glass and silicon containing compounds

    International Nuclear Information System (INIS)

    Irmer, K.

    1979-01-01

    A radiometric analyzer is described working on the principle of the thermal neutrons transfere. The device consists of two units: of the measuring gage into which the samples to be measured, are introduced; and of the measuring disk where the sygnals from the gage are processed. The measuring gage consists of the isotopic neutron source having the neutrons yield of 10 7 neutron/sec; BE 3 - scintillation counter and shield. The sample measured has a shape of cylinder and surrounds the counter. The neutron source is located in the paraffin moderator. The moderator with the neutron source in it, is rotating around a sample measured and, due to the rotation of the neutron source, uniform average neutron flux in the sample is obtained. Effective length of the proportional counter is limited by the cadmium neutron absorbers. Due to such design of the analyzer, unevenness of the radiation level of the sample measured do not affect measurement accuracy. The thermal neutrons transfer affects through the neutros capture by boron atoms and elastic interaction with the hydrogen atoms nuclei. Influence of hydrogen can be taken into account if the chemical composition of the boron containing compound is known. Due to simplicity, the device described is handy for industrial application. In the industrial conditions the device is repaid after 4 years of continious exploitation. Accuracy of measurements by this device is of 0.05% with time of measurement up to one minute [ru

  6. Use of a cranium-vessel determined by means of compound analysis

    International Nuclear Information System (INIS)

    Leboreiro, I.; Pijoan, C.M.; Mansilla, J.; Bosch, P.

    2004-01-01

    Many human remains as bones, skin, teeth and others, were used in pre-hispanic cultures as tools or ritual objects. A human cranial vault filed in the Direccion de Antropologia Fisica presented particular and interesting cultural modifications. There are twelve drills used to restore by sewing the crane, in this way the piece resembles a pot. It has been established that it comes from North Mexico where such restoration work has been reported (Aveleyra, 1956) for containers made of vegetables (guaje). As the utilization of this kind of archaeological remain is unknown, the study of dust samples from the inside and the outside of the crane should provide hints on the products stored into it. In this study we present the X-ray diffraction results which show that the outer dusts are mainly constituted by albite, andesite and quartz, whereas in the inside the substances were mainly aluminosilicates and magnesium compounds. Hence, most probably, this crane was not used as a conventional container and it is linked to the concoction of magnesium and aluminosilicates containing products. This conclusion has to be correlated to that even nowadays, in both alternative and conventional medicine. (Author) 7 refs., 7 figs

  7. Determination of Nerve Fiber Diameter Distribution From Compound Action Potential: A Continuous Approach.

    Science.gov (United States)

    Un, M Kerem; Kaghazchi, Hamed

    2018-01-01

    When a signal is initiated in the nerve, it is transmitted along each nerve fiber via an action potential (called single fiber action potential (SFAP)) which travels with a velocity that is related with the diameter of the fiber. The additive superposition of SFAPs constitutes the compound action potential (CAP) of the nerve. The fiber diameter distribution (FDD) in the nerve can be computed from the CAP data by solving an inverse problem. This is usually achieved by dividing the fibers into a finite number of diameter groups and solve a corresponding linear system to optimize FDD. However, number of fibers in a nerve can be measured sometimes in thousands and it is possible to assume a continuous distribution for the fiber diameters which leads to a gradient optimization problem. In this paper, we have evaluated this continuous approach to the solution of the inverse problem. We have utilized an analytical function for SFAP and an assumed a polynomial form for FDD. The inverse problem involves the optimization of polynomial coefficients to obtain the best estimate for the FDD. We have observed that an eighth order polynomial for FDD can capture both unimodal and bimodal fiber distributions present in vivo, even in case of noisy CAP data. The assumed FDD distribution regularizes the ill-conditioned inverse problem and produces good results.

  8. Determination of Volatile Compounds in Four Commercial Samples of Japanese Green Algae Using Solid Phase Microextraction Gas Chromatography Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Masayoshi Yamamoto

    2014-01-01

    Full Text Available Green algae are of great economic importance. Seaweed is consumed fresh or as seasoning in Japan. The commercial value is determined by quality, color, and flavor and is also strongly influenced by the production area. Our research, based on solid phase microextraction gas chromatography mass spectrometry (SPME-GC-MS, has revealed that volatile compounds differ intensely in the four varieties of commercial green algae. Accordingly, 41 major volatile compounds were identified. Heptadecene was the most abundant compound from Okayama (Ulva prolifera, Tokushima (Ulva prolifera, and Ehime prefecture (Ulva linza. Apocarotenoids, such as ionones, and their derivatives were prominent volatiles in algae from Okayama (Ulva prolifera and Tokushima prefecture (Ulva prolifera. Volatile, short chained apocarotenoids are among the most potent flavor components and contribute to the flavor of fresh, processed algae, and algae-based products. Benzaldehyde was predominant in seaweed from Shizuoka prefecture (Monostroma nitidum. Multivariant statistical analysis (PCA enabled simple discrimination of the samples based on their volatile profiles. This work shows the potential of SPME-GC-MS coupled with multivariant analysis to discriminate between samples of different geographical and botanical origins and form the basis for development of authentication methods of green algae products, including seasonings.

  9. Determination of volatile compounds in four commercial samples of Japanese green algae using solid phase microextraction gas chromatography mass spectrometry.

    Science.gov (United States)

    Yamamoto, Masayoshi; Baldermann, Susanne; Yoshikawa, Keisuke; Fujita, Akira; Mase, Nobuyuki; Watanabe, Naoharu

    2014-01-01

    Green algae are of great economic importance. Seaweed is consumed fresh or as seasoning in Japan. The commercial value is determined by quality, color, and flavor and is also strongly influenced by the production area. Our research, based on solid phase microextraction gas chromatography mass spectrometry (SPME-GC-MS), has revealed that volatile compounds differ intensely in the four varieties of commercial green algae. Accordingly, 41 major volatile compounds were identified. Heptadecene was the most abundant compound from Okayama (Ulva prolifera), Tokushima (Ulva prolifera), and Ehime prefecture (Ulva linza). Apocarotenoids, such as ionones, and their derivatives were prominent volatiles in algae from Okayama (Ulva prolifera) and Tokushima prefecture (Ulva prolifera). Volatile, short chained apocarotenoids are among the most potent flavor components and contribute to the flavor of fresh, processed algae, and algae-based products. Benzaldehyde was predominant in seaweed from Shizuoka prefecture (Monostroma nitidum). Multivariant statistical analysis (PCA) enabled simple discrimination of the samples based on their volatile profiles. This work shows the potential of SPME-GC-MS coupled with multivariant analysis to discriminate between samples of different geographical and botanical origins and form the basis for development of authentication methods of green algae products, including seasonings.

  10. Determinants of the Sensory Quality of Półgęsek in Relation to Volatile Compounds and Chemical Composition

    Directory of Open Access Journals (Sweden)

    Nowicka Katarzyna

    2017-12-01

    Full Text Available The objective of this study was to determine the sensory quality of a specific Polish traditional product made from cured and then smoked goose meat (półgęsek in relation to its volatile compounds and chemical composition. In general, the examined samples contained 66.2% water, 12.2% fat, 17.9% protein, 1.8% connective tissue, and 2.3% NaCl. Moreover, 47 volatile compounds were identified and quantified. The typical decomposition products derived from lipid oxidation, amino acid degradation, carbohydrate fermentation and microbial esterification were the main volatiles detected in all the samples. The volatiles generated by the smoking process and the ones originating from spices were also observed. The results of the sensory evaluation indicated that all the samples of the analyzed products were characterized by a high overall quality. Results of the Principal Component Analysis (PCA showed, however, that specific groups of products have their own unique sensory profile. Additionally, the sensory analysis confirmed the significant role of the chemical composition and volatile compounds in the development of the overall quality of półgęsek.

  11. Determination of the enthalpy of formation of Ni-Al intermetallic compounds using differential scanning calorimetry technique

    International Nuclear Information System (INIS)

    Kubaski, Evaldo Toniolo; Capocchi, Jose Deodoro Trani; Cintho, Osvaldo Mitsuyuki

    2010-01-01

    The compositions Ni20Al80, Ni25Al75, Ni40Al60, Ni50Al50, Ni60Al40 and Ni75Al25 (at. %) were heated in a calibrated thermal analysis equipment. All runs were conducted at a heating rate of 10 deg C/min under a dynamic argon atmosphere. Each composition was heated until the completion of the corresponding exothermic reaction responsible for intermetallic compound formation, and, also heated to 1480 deg C. The products obtained were characterized using X ray diffraction in order to identify the intermetallic compounds that were synthesized. Moreover, the results were evaluated using variance analysis. As a result, enthalpies of formation of Ni 2 Al 3 and Ni 3 Al compounds were determined by means of this methodology. Experimental values were 167 kJ/mol and 93 kJ/mol for Ni 2 Al 3 and Ni 3 Al, respectively. The former is 18% lower than the value found on literature, while the latter is 6% greater. (author)

  12. HPLC-QTOF-MS method for quantitative determination of active compounds in an anti-cellulite herbal compress

    Directory of Open Access Journals (Sweden)

    Ngamrayu Ngamdokmai

    2017-08-01

    Full Text Available A herbal compress used in Thai massage has been modified for use in cellulite treatment. Its main active ingredients were ginger, black pepper, java long pepper, tea and coffee. The objective of this study was to develop and validate an HPLCQTOF-MS method for determining its active compounds, i.e., caffeine, 6-gingerol, and piperine in raw materials as well as in the formulation together with the flavouring agent, camphor. The four compounds were chromatographically separated. The analytical method was validated through selectivity, intra-, inter day precision, accuracy and matrix effect. The results showed that the herbal compress contained caffeine (2.16 mg/g, camphor (106.15 mg/g, 6-gingerol (0.76 mg/g, and piperine (4.19 mg/g. The chemical stability study revealed that herbal compresses retained >80% of their active compounds after 1 month of storage at ambient conditions. Our method can be used for quality control of the herbal compress and its raw materials.

  13. Extraction and GC determination of volatile aroma compounds from extracts of three plant species of the Apiaceae family

    Science.gov (United States)

    Stan, M.; Soran, M. L.; Varodi, C.; Lung, I.; Copolovici, L.; MǎruÅ£oiu, C.

    2013-11-01

    Parsley (Petroselinum crispum), dill (Anethum graveolens) and celery (Apium graveolens), three aromatic plants belonging to the Apiaceae (Umbelliferae) botanical family, were selected as sources of essential or volatile oils. Essential oils are composed of a large diversity of volatile aroma compounds. Plant-derived essential oils and extracts have long been used as natural agents in food preservation, pharmaceuticals and medicinal therapies. In the present study, the plant extracts from leaves of parsley, dill and celery, were obtained by maceration, ultrasound-assisted extraction and microwave-assisted extraction. All extractions were performed at 30°C, using different solvents (ethanol, diethyl ether, n-hexane) and solvent mixtures (1:1, v/v). The most effective solvent system for the extraction of volatile aroma compounds was diethyl ether - n-hexane (1:1, v/v). Extraction efficiency and determination of aroma volatiles were performed by GC-FID and GC-MS, respectively. The major volatile compounds present in plant extracts were myristicin, α-phellandrene, β-phellandrene, 1,3,8-p-menthatriene, apiol, dill ether and allyl phenoxyacetate.

  14. Direct sample introduction-gas chromatography-mass spectrometry for the determination of haloanisole compounds in cork stoppers.

    Science.gov (United States)

    Cacho, J I; Nicolás, J; Viñas, P; Campillo, N; Hernández-Córdoba, M

    2016-12-02

    A solventless analytical method is proposed for analyzing the compounds responsible for cork taint in cork stoppers. Direct sample introduction (DSI) is evaluated as a sample introduction system for the gas chromatography-mass spectrometry (GC-MS) determination of four haloanisoles (HAs) in cork samples. Several parameters affecting the DSI step, including desorption temperature and time, gas flow rate and other focusing parameters, were optimized using univariate and multivariate approaches. The proposed method shows high sensitivity and minimises sample handling, with detection limits of 1.6-2.6ngg -1 , depending on the compound. The suitability of the optimized procedure as a screening method was evaluated by obtaining decision limits (CCα) and detection capabilities (CCβ) for each analyte, which were found to be in 6.9-11.8 and 8.7-14.8ngg -1 , respectively, depending on the compound. Twenty-four cork samples were analysed, and 2,4,6-trichloroanisole was found in four of them at levels between 12.6 and 53ngg -1 . Copyright © 2016 Elsevier B.V. All rights reserved.

  15. Determination of adiabatic temperature change in MnFe(P,Ge) compounds with pulse-field method

    International Nuclear Information System (INIS)

    Trung, N T; Tegus, O; Cam Thanh, D T; Buschow, K H J; Brueck, E; Klaasse, J C P

    2010-01-01

    Fast magnetic measurements performed by means of a 20 T pulse-field magnet provide a good approach for directly monitoring the magnetocaloric effect of the MnFe(P,Ge) compounds. Based on the comparison of magnetization curves obtained either in an adiabatic or isothermal process, we propose that the method introduced by Levitin et al is applicable to determine the adiabatic temperature change for an equivalent field change in first-order magnetic transition materials. More strikingly, experimental results confirm that the first-order nature of the transition in MnFe(P,Ge) alloys is not a limiting factor to the operation frequency of a magnetic refrigerator.

  16. Determination of metallic impurities in nuclearly pure uranium compounds by electrothermal spectrophotometry

    International Nuclear Information System (INIS)

    Franco, M.B.

    1986-01-01

    Atomic absorption spectrometry, with electrothermal atomization, has been used for the determination of Al, Cd, Cr, Fe, Mn and Ni in uranium oxide standards. The analysis were performed without sample dissolution and without uranium chemical separation. This technique is adequate for the qualification of nuclearly pure uranium, according to the standard specifications. (Author) [pt

  17. Adhesives, fillers & potting compounds: Special report molecular weight determinations of dimethypolysiloxane polymers

    Energy Technology Data Exchange (ETDEWEB)

    Luthey, Z.A.

    1968-09-03

    Using a Mechrolab Vapor Phase Osmometer and a Hallikainen Automatic Membrane Osmometer the number-average molecular weight of two samples of dimethylpolysiloxane - 2300 and 8000 cstk - as well as samples made by mixing the two previously mentioned materials were determined.

  18. "Cork taint" responsible compounds. Determination of haloanisoles and halophenols in cork matrix: A review.

    Science.gov (United States)

    Tarasov, Andrii; Rauhut, Doris; Jung, Rainer

    2017-12-01

    Analytical methods of haloanisoles and halophenols quantification in cork matrix are summarized in the current review. Sample-preparation and sample-treatment techniques have been compared and discussed from the perspective of their efficiency, time- and extractant-optimization, easiness of performance. Primary interest of these analyses usually addresses to 2,4,6-trichloroanisole (TCA), which is a major wine contaminant among haloanisoles. Two concepts of TCA determination are described in the review: releasable TCA and total TCA analyses. Chromatographic, bioanalytical and sensorial methods were compared according to their application in the cork industry and in scientific investigations. Finally, it was shown that modern analytical techniques are able to provide required sensitivity, selectivity and repeatability for haloanisoles and halophenols determination. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Fragile Thermodynamic Order

    International Nuclear Information System (INIS)

    Bernhoeft, N.; Lander, G.H.; Colineau, E.

    2003-01-01

    An asymmetric shift in the position of the magnetic Bragg peak with respect to the fiducial lattice has been observed by resonant X-ray scattering in a diverse series of antiferromagnetic compounds. This apparent violation of Bragg's law is interpreted in terms of a dynamically phased order parameter. We demonstrate the use of this effect as a novel probe of fragile or dynamic thermodynamic order in strongly correlated electronic systems. In particular, fresh light is shed on the paradoxical situation encountered in URu 2 Si 2 where the measured entropy gain on passing through T Neel is incompatible with the ground state moment estimated by neutron diffraction. The intrinsic space-time averaging of the probe used to characterise the thermodynamic macroscopic state may play a crucial and previously neglected role. In turn, this suggests the further use of resonant X-ray scattering in investigations of systems dominated by quantum fluctuations. (author)

  20. Miniaturised sample preparation method for the multiresidual determination of regulated organohalogenated pollutants and related compounds in wild bird eggs.

    Science.gov (United States)

    Roscales, Jose L; Vicente, Alba; Ramos, Lourdes; Jiménez, Begoña

    2017-08-01

    A simplified, miniaturised matrix solid-phase dispersion (MSPD)-based method allowing the simultaneous extraction and purification of contaminants belonging to selected families of regulated persistent organic pollutants (POPs), i.e. polychlorinated biphenyls (PCBs), organochlorine pesticides (OCPs) and penta- to octa-polybrominated diphenyl ethers (PBDEs), and related contaminants of emerging concern, such as deca-BDE and Dechlorane Plus (DP), has been proposed. Wild bird eggs were used as biotic fat-containing model matrices. Once optimised, the procedure allowed sample preparation to be accomplished within 30 min, in a single step, and with minimal sample and reagent consumption and waste generation. These features contributed to speeding up and greening the analytical process as compared to the large-scale multistep procedures for these types of analyses. The method was combined with gas chromatography-quadrupole mass spectrometry (GC-qMS) for PCB and OCP analysis and with GC-negative ion chemical ionisation-quadrupole mass spectrometry (NCI-qMS) for PBDE and DP determination. The complete analytical method provided satisfactory recoveries of the target compounds (above 83% for all analytes, except for PBDE 209, 63%), although as small an amount of sample as 0.300 g was used. The repeatability of the complete procedure was less than 16% (with the only exception for PCB 153, which looked to be affected by an interference). The limits of detection were in all cases lower than 34 pg g -1 dry weight (as calculated for real samples), demonstrating the feasibility of the proposed procedure for accurate determination of the target compounds in biological samples. The proposed procedure was applied to the analysis of the target POPs in unhatched eggs of wild bird species. Graphical abstract Scheme of the miniaturised methodology proposed for environmental monitoring of POPs and related compounds in wild bird eggs.

  1. Pulsed amperometric detection at glassy carbon electrodes: A new waveform for sensitive and reproducible determination of electroactive compounds.

    Science.gov (United States)

    Nardiello, Donatella; Palermo, Carmen; Natale, Anna; Quinto, Maurizio; Centonze, Diego

    2015-09-24

    In this work, the application of a new pulsed amperometric detection (PAD) waveform at a glassy carbon electrode, operating in typical chromatographic mobile phases, is proposed for the sensitive and reproducible determination of arylethanolaminic and phenolic moiety based compounds (e.g. beta-agonists and polyphenols). Preliminary experiments by cyclic voltammetry were carried out to investigate the electrochemical behaviour and to select the detection and cleaning electrode potentials. The proposed potential-time profile was designed to prevent the carbon electrode fouling under repeated analyses, thus ensuring a reproducible and sensitive quantitative determination, without the need of any mechanical or chemical electrode cleaning procedure. The waveform electrochemical parameters, including detection and delay times, were optimized in terms of sensitivity, limit of detection and response stability. The optimized waveform allowed the sensitive and stable detection of model compounds, such as clenbuterol and caffeic acid, that showed detection limits of 0.1 μg L(-1) and 14 μg L(-1), quantification limits of 0.4 μg L(-1) and 46 μg L(-1), and linearity up to 100 μg L(-1) (r = 0.9993) and 10 mg L(-1) (r = 0.9998), respectively. Similar results were obtained for other compounds of the same classes, with precision values under repeatability conditions ranging from 3.0 to 5.9%. The proposed method can be then considered as an excellent alternative to the post-column detection of beta-agonists, phenols and polyphenols. Copyright © 2015 Elsevier B.V. All rights reserved.

  2. Determination of naphthalene-derived compounds in apples by ultra-high performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Esparza, X; Moyano, E; Cosialls, J R; Galceran, M T

    2013-06-11

    Naphthylacetic acid, naphthyloxy acetic acid and naphthylacetamide belong to a group of synthetic substances known as "auxin-like" compounds which are used as growth regulators in vegetables and fruits due to their structure similarities with the indoleacetic acid, the most important plant auxin. This paper reports a selective, sensitive and fast ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method for the determination of naphthylacetamide (NAD) and the isomers (α and β) of naphthylacetic acid (NAA) and naphthyloxy acetic (NOA) acid in apple samples. A baseline separation between the respective isomers was achieved using an RP-Amide column with gradient elution. The UHPLC-MS/MS method developed, using electrospray and selected reaction monitoring (SRM) acquisition mode led to a reliable determination of these family of compounds in apple samples at low quantitation levels, down to 1.0 μg kg(-1) and 0.25 μg kg(-1) respectively. For confirmation of NAA accurate mass measurement is proposed giving at these conditions quantitation limits of 10 μg kg(-1) for this compound. The UHPLC-MS/MS method developed was used for the analysis of apple samples harvested in three different apple fields from Lleida (Spain) during the blooming period. NAD and NAA were found in samples collected during 4-5 weeks after application at concentrations between the quantification limits and 43 μg kg(-1) and 24 μg kg(-1), respectively. Copyright © 2013 Elsevier B.V. All rights reserved.

  3. Analysis of uranium and of some of its compounds and alloys. Copper spectrophotometric determination

    International Nuclear Information System (INIS)

    Copper determination in uranium, uranium oxides (UO 2 , UO 3 , U 3 O 8 ), ammonium diuranate, U-Al-Fe alloy (700 ppm Al and 300 ppm Fe) and U-Mo alloy (1.1 percent Mo) by acid dissolution reduction of copper by hydroxylamine hydrochloride and formation of a complex with diquinolyle-2,2' amyl alcohol (pH value 6 to 7) and spectrophotometry at 550 nm. The method is applicable for copper content between 5 to 40 ppm in respect of uranium contained in the material [fr

  4. Analytical protocols for the determination of sulphur compounds characteristic of the metabolism of Chlorobium limicola

    Directory of Open Access Journals (Sweden)

    A. Aliboni

    2015-09-01

    Full Text Available Chlorobium limicola belongs to the green sulphur bacteria that has a potential for technological applications such as biogas clean up oxidising hydrogen sulphide to elemental sulphur through photosynthetic process. In the present work, analytical methods are described for the determination of different sulphur species in C. limicola cultures – sulphide by GC-FPD, sulphate by ionic HPLC and elemental sulphur by RP HPLC. The latter method eliminates the need for chloroform extraction of water suspensions of elemental sulphur. Data from sulphide and elemental sulphur analyses have been compared with ones coming from more traditional analytical methodologies.

  5. Determination of volatile organic compounds in eucalyptus fast pyrolysis bio-oil by full evaporation headspace gas chromatography.

    Science.gov (United States)

    Kosinski Lima, Nathalya; Romualdo Lopes, André; Gimenes Guerrero, Palimecio; Itsuo Yamamoto, Carlos; Augusto Hansel, Fabricio

    2018-01-01

    This paper reports a full evaporation (FE) headspace gas chromatographic (HS-GC) method for the determination of the volatile organic compounds (VOCs) in bio-oil (i.e. methanol, ethanol, acetone, acetic acid and furfural). The method uses a 4μL sample of bio-oil in a headspace vial (ca. 20mL). Complete evaporation of the compounds was achieved after seven minutes at 90°C. The method showed good precision and accuracy for methanol, ethanol, acetone and acetic acid. The recovery of furfural was low (74.3%). The results showed that the protocol can be applied for the determination of methanol, ethanol, acetone and acetic acid in bio-oil. Detection limits ranged from 0.13 to 0.16μg. Acetic acid was the dominant analyte in the heavy bio-oil and light bio-oil analysis (113. 3 and 85.1µgmg -1 , respectively), followed by methanol, ethanol, and acetone. The polymerisation of furfural was suspected as the cause of its poor quantification. Copyright © 2017 Elsevier B.V. All rights reserved.

  6. Multi-residue determination of 47 organic compounds in water, soil, sediment and fish-Turia River as case study.

    Science.gov (United States)

    Carmona, Eric; Andreu, Vicente; Picó, Yolanda

    2017-11-30

    A sensitive and reliable method based on solid-liquid extraction (SLE) using McIlvaine-Na 2 EDTA buffer (pH=4.5)-methanol and solid-phase extraction (SPE) clean up prior to ultra-high-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) was applied to determine 47 organic contaminants in fish, soil and sediments. The SPE procedure to clean-up the extracts was also used as extraction method to determine these compounds in water. Recoveries ranged from 38 to 104% for all matrices with RSDsfish and 0.3-26ng/L for water. Furthermore, the proposed method was compared to QuEChERS (widely used for environmental matrices) that involves extraction with buffered acetonitrile (pH 5.5) and dispersive SPE clean-up. The results obtained (recoveries>50% for 36 compounds in front of 9, matrix effectfish, bisphenol A (33ngg -1 ) or sulfamethoxazole (13ngg -1 ). Copyright © 2017 Elsevier B.V. All rights reserved.

  7. Ionic Liquid Crystals Modifier for Selective Determination of Terazosin Antihypertensive Drug in Presence of Common Interference Compounds

    Directory of Open Access Journals (Sweden)

    Nada F. Atta

    2017-01-01

    Full Text Available Electrochemical sensor was fabricated based on carbon paste electrode modified with an ionic liquid crystal ILC (2-chloro-1,3-dimethyl-imidazolidinium hexafluorophosphate in presence of sodium dodecyl sulfate for the selective electrochemical determination of Terazosin (TZ in presence of common interference compounds. The electrode performance was compared in presence of other ionic liquids ILs (1-Butyl-4-methyl pyridinium tetrafluoroborate and (1-n-Hexyl-3-methyl imidazolium tetrafluoroborate. Ultrasensitive determination of Terazosin HCl at the ILC modified electrode in the linear dynamic ranges of 0.002 to 0.09 μmol·L−1 and 0.2 to 30 μmol·L−1 with correlation coefficients 0.996 and 0.995 and LODs 1.69 × 10−11 mol·L−1 and 6.43 × 10−9 mol·L−1, respectively, were obtained. Selective determination of TZ in presence of uric acid and ascorbic acid and simultaneous determination of binary mixtures of TZ/dopamine, TZ/paracetamol and TZ/Morphine were also determined successfully using the modified sensor.

  8. Development of an Analytical Procedure for the Determination of Multiclass Compounds for Forensic Veterinary Toxicology.

    Science.gov (United States)

    Sell, Bartosz; Sniegocki, Tomasz; Zmudzki, Jan; Posyniak, Andrzej

    2018-04-01

    Reported here is a new analytical multiclass method based on QuEChERS technique, which has proven to be effective in diagnosing fatal poisoning cases in animals. This method has been developed for the determination of analytes in liver samples comprising rodenticides, carbamate and organophosphorus pesticides, coccidiostats and mycotoxins. The procedure entails addition of acetonitrile and sodium acetate to 2 g of homogenized liver sample. The mixture was shaken intensively and centrifuged for phase separation, which was followed by an organic phase transfer into a tube containing sorbents (PSA and C18) and magnesium sulfate, then it was centrifuged, the supernatant was filtered and analyzed by liquid chromatography tandem mass spectrometry. A validation of the procedure was performed. Repeatability variation coefficients forensic toxicology cases.

  9. Anti-methicillin Resistant Staphylococcus aureus Compound Isolation from Halophilic Bacillus amyloliquefaciens MHB1 and Determination of Its Mode of Action Using Electron Microscope and Flow Cytometry Analysis.

    Science.gov (United States)

    Jeyanthi, Venkadapathi; Velusamy, Palaniyandi

    2016-06-01

    The aim of this study was to purify, characterize and evaluate the antibacterial activity of bioactive compound against methicillin-resistant Staphylococcus aureus (MRSA). The anti-MRSA compound was produced by a halophilic bacterial strain designated as MHB1. The MHB1 strain exhibited 99 % similarity to Bacillus amyloliquefaciens based on 16S rRNA gene analysis. The culture conditions of Bacillus amyloliquefaciens MHB1 were optimized using nutritional and environmental parameters for enhanced anti-MRSA compound production. The pure bioactive compound was isolated using silica gel column chromatography and Semi-preparative High-performance liquid chromatography (Semi-preparative HPLC). The Thin layer chromatography, Fourier transform infrared spectroscopy and proton NMR ((1)H NMR) analysis indicated the phenolic nature of the compound. The molecular mass of the purified compound was 507 Da as revealed by Liquid chromatography-mass spectrometry (LC-MS) analysis. The compound inhibited the growth of MRSA with minimum inhibitory concentration (MIC) of 62.5 µg mL(-1). MRSA bacteria exposed to 4× MIC of the compound and the cell viability was determined using flow cytometric analysis. Scanning electron microscope and Transmission electron microscope analysis was used to determine the ultrastructural changes in bacteria. This is the first report on isolation of anti-MRSA compound from halophilic B. amyloliquefaciens MHB1 and could act as a promising biocontrol agent.

  10. Determination of trace lithium in uranium compounds by adsorption on activated alumina using a micro-column method.

    Science.gov (United States)

    Luo, Ming-Biao; Li, Bo-Ping; Yang, Zhi; Liu, Wei; Sun, Yu-Zhen

    2008-08-01

    A novel method using a micro-column packed with active alumina as solid phase was proposed for separation of trace lithium from uranium compounds prior to determination. The method is based on a preliminary chromatographic separation of the total amount of uranium. This separation involves passing the solution containing sodium carbonate through active alumina and then eluting the trace lithium retained by the solid phase with a solution of sulfuric acid. Two modes, off-line and on-line micro-column preconcentration, were performed. In conjunction with atomic absorption spectrometry, this on-line preconcentration technique allows a determination of lithium at 10(-9) level. Both off-line and on-line mode operation conditions were investigated in separation and determination of trace lithium by micro-column method (length of column bed, flow rate, etc.). The adsorption capacity of activated alumina was found to be 343 microg g(-1) for lithium. Under the optimal operation condition, the detection limit (DL) of on-line preconcentration corresponding to three times the standard deviation of the blank (S/N = 3) was found to be 1.3 ng mL(-1) and the RSD of this method is 3.32% (n = 5). The on-line calibration graph was linear over the range 20 - 200 ng mL(-1). A good preconcentration factor 820 was achieved by experiment under the on-line mode. The developed method was applied to the analysis of trace lithium in nuclear grade uranium compounds.

  11. Role of natural dissolved organic compounds in determining the concentrations of americium in natural waters

    International Nuclear Information System (INIS)

    Nelson, D.M.; Orlandini, K.A.

    1985-01-01

    Concentrations of 241 Am, both in solution and bound to suspended particulate matter, have been measured in several North American lakes. Dissolved concentrations vary from 0.4 μBq/L to 85 μBq/L. The 241 Am in these lakes originated solely from global fallout and hence entered all lakes in the same physiocochemical form. The observed differences in solubility behavior must, therefore, be attributable to chemical and/or hydrological differences among the lakes. Concentrations of dissolved 241 Am are highly correlated with the corresponding concentrations of /sup 239, 240/Pu(III,IV), suggesting that a common factor is responsible for maintaining both in solution. The K/sub D/ values for 241 Am and /sup 239, 240/Pu(III,IV) are highly correlated with the concentrations of dissolved organic carbon (DOC) in the waters, suggesting that the common factor is the formation of soluble complexes with natural DOC for both elements. This hypothesis was tested in a series of laboratory experiments in which the DOC from several of the lakes was isolated by ultrafiltration. Plots of K/sub D/, as a function of DOC concentration, show K/sub D/ to be very high (approx.10 6 ) at low DOC concentrations. Above critical concentrations (a few mg/L DOC) the K/sub D/ values begin a progressive decrease with increasing DOC. We conclude that in most surface waters, the dissolved 241 Am concentration is regulated by an adsorption/desorption equilibrium with the sediments (and suspended solids) and the value of K/sub D/ that characterizes this equilibrium is largely determined by the concentration of natural DOC in the water. 11 refs., 3 figs., 2 tabs

  12. The Determination of Pesticidal and Non-Pesticidal Organotin Compounds by in situ Ethylation and Capillary Gas Chromatography with Pulsed Flame Photometric Detection

    Science.gov (United States)

    The concurrent determination of pesticidal and non-pesticidal organotin compounds in several water matrices, using a simultaneous in situ ethylation and liquid-liquid extraction followed by splitless injection mode capillary gas chromatography with pulsed flame photometric detect...

  13. The Determination of Pesticidal and Non-Pesticidal Organotin Compounds in Water Matrices by in situ Ethylation and Gas Chromatography with Pulsed Flame Photometric Detection

    Science.gov (United States)

    The concurrent determination of pesticidal and non-pesticidal organotin compounds in several water matrices, using a simultaneous in situ ethylation and liquid-liquid extraction followed by splitless injection mode capillary gas chromatography with pulsed flame photometric detect...

  14. Chemistry of Volatile Organic Compounds in the Los Angeles basin: Nighttime Removal of Alkenes and Determination of Emission Ratios

    Science.gov (United States)

    de Gouw, J. A.; Gilman, J. B.; Kim, S.-W.; Lerner, B. M.; Isaacman-VanWertz, G.; McDonald, B. C.; Warneke, C.; Kuster, W. C.; Lefer, B. L.; Griffith, S. M.; Dusanter, S.; Stevens, P. S.; Stutz, J.

    2017-11-01

    We reanalyze a data set of hydrocarbons in ambient air obtained by gas chromatography-mass spectrometry at a surface site in Pasadena in the Los Angeles basin during the NOAA California Nexus study in 2010. The number of hydrocarbon compounds quantified from the chromatograms is expanded through the use of new peak-fitting data analysis software. We also reexamine hydrocarbon removal processes. For alkanes, small alkenes, and aromatics, the removal is determined by the reaction with hydroxyl (OH) radicals. For several highly reactive alkenes, the nighttime removal by ozone and nitrate (NO3) radicals is also significant. We discuss how this nighttime removal affects the determination of emission ratios versus carbon monoxide (CO) and show that previous estimates based on nighttime correlations with CO were too low. We analyze model output from the Weather Research and Forecasting-Chemistry model for hydrocarbons and radicals at the Pasadena location to evaluate our methods for determining emission ratios from the measurements. We find that our methods agree with the modeled emission ratios for the domain centered on Pasadena and that the modeled emission ratios vary by 23% across the wider South Coast basin. We compare the alkene emission ratios with published results from ambient measurements and from tunnel and dynamometer studies of motor vehicle emissions. We find that with few exceptions the composition of alkene emissions determined from the measurements in Pasadena closely resembles that of motor vehicle emissions.

  15. Full evaporation headspace gas chromatography for sensitive determination of high boiling point volatile organic compounds in low boiling matrices.

    Science.gov (United States)

    Mana Kialengila, Didi; Wolfs, Kris; Bugalama, John; Van Schepdael, Ann; Adams, Erwin

    2013-11-08

    Determination of volatile organic components (VOC's) is often done by static headspace gas chromatography as this technique is very robust and combines easy sample preparation with good selectivity and low detection limits. This technique is used nowadays in different applications which have in common that they have a dirty matrix which would be problematic in direct injection approaches. Headspace by nature favors the most volatile compounds, avoiding the less volatile to reach the injector and column. As a consequence, determination of a high boiling solvent in a lower boiling matrix becomes challenging. Determination of VOCs like: xylenes, cumene, N,N-dimethylformamide (DMF), dimethyl sulfoxide (DMSO), N,N-dimethylacetamide (DMA), N-methyl-2-pyrrolidone (NMP), 1,3-dimethyl-2-imidazolidinone (DMI), benzyl alcohol (BA) and anisole in water or water soluble products are an interesting example of the arising problems. In this work, a headspace variant called full evaporation technique is worked out and validated for the mentioned solvents. Detection limits below 0.1 μg/vial are reached with RSD values below 10%. Mean recovery values ranged from 92.5 to 110%. The optimized method was applied to determine residual DMSO in a water based cell culture and DMSO and DMA in tetracycline hydrochloride (a water soluble sample). Copyright © 2013 Elsevier B.V. All rights reserved.

  16. Heats of formation of phosphorus compounds determined by current methods of computational quantum chemistry

    Science.gov (United States)

    Haworth, Naomi L.; Bacskay, George B.

    2002-12-01

    The heats of formation of a range of phosphorus containing molecules (P2, P4, PH, PH2, PH3, P2H2, P2H4, PO, PO2, PO3, P2O, P2O2, HPO, HPOH, H2POH, H3PO, HOPO, and HOPO2) have been determined by high level quantum chemical calculations. The equilibrium geometries and vibrational frequencies were computed via density functional theory, utilizing the B3LYP/6-31G(2df,p) functional and basis set. Atomization energies were obtained by the application of ab initio coupled cluster theory with single and double excitations from (spin)-restricted Hartree-Fock reference states with perturbative correction for triples [CCSD(T)], in conjunction with cc-pVnZ basis sets (n=T, Q, 5) which include an extra d function on the phosphorus atoms and diffuse functions on the oxygens, as recommended by Bauschlicher [J. Phys. Chem. A 103, 11126 (1999)]. The valence correlated atomization energies were extrapolated to the complete basis limit and corrected for core-valence (CV) correlation and scalar relativistic effects, as well as for basis set superposition errors (BSSE) in the CV terms. This methodology is effectively the same as the one adopted by Bauschlicher in his study of PO, PO2, PO3, HPO, HOPO, and HOPO2. Consequently, for these molecules the results of this work closely match Bauschlicher's computed values. The theoretical heats of formation, whose accuracy is estimated as ranging from ±1.0 to ±2.5 kcal mol-1, are consistent with the available experimental data. The current set of theoretical data represent a convenient benchmark, against which the results of other computational procedures, such as G3, G3X, and G3X2, can be compared. Despite the fact that G3X2 [which is an approximation to the quadratic CI procedure QCISD(T,Full)/G3Xlarge] is a formally higher level theory than G3X, the heats of formation obtained by these two methods are found to be of comparable accuracy. Both reproduce the benchmark heats of formation on the average to within ±2 kcal mol-1 and, for these

  17. Static liquid permeation cell method for determining the migration parameters of low molecular weight organic compounds in polyethylene terephthalate.

    Science.gov (United States)

    Song, Yoon S; Koontz, John L; Juskelis, Rima O; Zhao, Yang

    2013-01-01

    The migration of low molecular weight organic compounds through polyethylene terephthalate (PET) films was determined by using a custom permeation cell assembly. Fatty food simulant (Miglyol 812) was added to the receptor chamber, while the donor chamber was filled with 1% and 10% (v/v) migrant compounds spiked in simulant. The permeation cell was maintained at 40°C, 66°C, 100°C or 121°C for up to 25 days of polymer film exposure time. Migrants in Miglyol were directly quantified without a liquid-liquid extraction step by headspace-GC-MS analysis. Experimental diffusion coefficients (DP) of toluene, benzyl alcohol, ethyl butyrate and methyl salicylate through PET film were determined. Results from Limm's diffusion model showed that the predicted DP values for PET were all greater than the experimental values. DP values predicted by Piringer's diffusion model were also greater than those determined experimentally at 66°C, 100°C and 121°C. However, Piringer's model led to the underestimation of benzyl alcohol (Áp = 3.7) and methyl salicylate (Áp = 4.0) diffusion at 40°C with its revised "upper-bound" Áp value of 3.1 at temperatures below the glass transition temperature (Tg) of PET (<70°C). This implies that input parameters of Piringer's model may need to be revised to ensure a margin of safety for consumers. On the other hand, at temperatures greater than the Tg, both models appear too conservative and unrealistic. The highest estimated Áp value from Piringer's model was 2.6 for methyl salicylate, which was much lower than the "upper-bound" Áp value of 6.4 for PET. Therefore, it may be necessary further to refine "upper-bound" Áp values for PET such that Piringer's model does not significantly underestimate or overestimate the migration of organic compounds dependent upon the temperature condition of the food contact material.

  18. Development and validation of RP-HPLC-UV/ Vis method for determination of phenolic compounds in several personal care products

    International Nuclear Information System (INIS)

    Mohammed Akkbik; Zaini Asim; Fasihuddin Ahmad

    2011-01-01

    A HPLC method with ultraviolet-visible spectrophotometry detection has been optimized and validated for the simultaneous determination of phenolic compounds, such as butylated hydroxyanisole (BHA) and butylated hydroxytoluene (BHT) as antioxidants, and octyl methyl cinnamate (OMC) as UVB-filter in several personal care products. The dynamic range was between 1 to 250 mg/ L with relative standard deviation less than 0.25 %, (n=4). Limit of detection for BHA, BHT and OMC were 0.196, 0.170 and 0.478 mg/ L, respectively. While limit of quantification for BHA, BHT and OMC were 0.593, 0.515 and 1.448 mg/ L, respectively. The recovery for BHA, BHT and OMC ranged from 92.1-105.9 %, 83.2-108.9 % and 87.3-103.7 %, respectively. The concentration ranges of BHA, BHT and OMC in 12 commercial personal care samples were 0.13-4.85, 0.16-2.30 and 0.12-65.5 mg/ g, respectively. The concentrations of phenolic compounds in these personal care samples were below than maximum allowable concentration in personal care formulation for example 0.0004 - 10 mg/ g, 0.002 - 5 mg/ g and up to 100 mg/ g for BHA, BHT and OMC, respectively. (author)

  19. Consolidating a Distributed Compound Management Capability into a Single Installation: The Application of Overall Equipment Effectiveness to Determine Capacity Utilization.

    Science.gov (United States)

    Green, Clive; Taylor, Daniel

    2016-12-01

    Compound management (CM) is a critical discipline enabling hit discovery through the production of assay-ready compound plates for screening. CM in pharma requires significant investments in manpower, capital equipment, repairs and maintenance, and information technology. These investments are at risk from external factors, for example, new technology rendering existing equipment obsolete and strategic site closures. At AstraZeneca, we faced the challenge of evaluating the number of CM sites required to support hit discovery in response to site closures and pressure on our operating budget. We reasoned that overall equipment effectiveness, a tool used extensively in the manufacturing sector, could determine the equipment capacity and appropriate number of sites. We identified automation downtime as the critical component governing capacity, and a connection between automation downtime and the availability of skilled staff. We demonstrated that sufficient production capacity existed in two sites to meet hit discovery demand without the requirement for an additional investment of $7 million in new facilities. In addition, we developed an automated capacity model that incorporated an extended working-day pattern as a solution for reducing automation downtime. The application of this solution enabled the transition to a single site, with an annual cost saving of $2.1 million. © 2015 Society for Laboratory Automation and Screening.

  20. Determination of quaternary ammonium compounds in seawater samples by solid-phase extraction and liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Bassarab, P; Williams, D; Dean, J R; Ludkin, E; Perry, J J

    2011-02-04

    A method for the simultaneous determination of two biocidal quaternary ammonium compounds; didecyldimethylammonium chloride (didecyldimethyl quat) and dodecylbenzyldimethylammonium chloride (benzyl quat), in seawater by solid phase extraction (SPE) followed by liquid chromatography-mass spectrometry (LC-MS) was developed. The optimised procedure utilised off-line extraction of the analytes from seawater using polymeric (Strata-X) SPE cartridges. Recoveries ranged from 80 to 105%, with detection limits at the low parts-per-trillion (ng/l) level for both analytes. To demonstrate sensitivity, environmental concentrations were measured at three different locations along the North East coast of England with measured values in the range 120-270ng/l. Copyright © 2010 Elsevier B.V. All rights reserved.

  1. Determination of Endocrine Disrupting Compounds in surface waters by means of chromatographic techniques coupled to mass spectrometry

    Directory of Open Access Journals (Sweden)

    M. Di Carro

    2011-01-01

    Full Text Available Two analytical methods were developed to study five endocrine disrupting compounds (4-n-nonylphenol, bisphenol A, estrone, 17β-estradiol and 17α-ethinylestradiol in waters. One method includes a fast liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS-MS analysis, while the second comprise a Stir Bar Sorptive Extraction (SBSE followed by a headspace derivatization and gaschromatography-mass spectrometry (GC-MS analysis. Passive samplers POCIS (Polar Organic Chemical Integrative Samplers were used as sampling and preconcentration steps in order to reach the very low levels of the analytes in environmental waters. Both methods were then applied to the determination of the analytes in different water samples.

  2. [Determination of six main components in compound theophylline tablet by convolution curve method after prior separation by column partition chromatography

    Science.gov (United States)

    Zhang, S. Y.; Wang, G. F.; Wu, Y. T.; Baldwin, K. M. (Principal Investigator)

    1993-01-01

    On a partition chromatographic column in which the support is Kieselguhr and the stationary phase is sulfuric acid solution (2 mol/L), three components of compound theophylline tablet were simultaneously eluted by chloroform and three other components were simultaneously eluted by ammonia-saturated chloroform. The two mixtures were determined by computer-aided convolution curve method separately. The corresponding average recovery and relative standard deviation of the six components were as follows: 101.6, 1.46% for caffeine; 99.7, 0.10% for phenacetin; 100.9, 1.31% for phenobarbitone; 100.2, 0.81% for theophylline; 99.9, 0.81% for theobromine and 100.8, 0.48% for aminopyrine.

  3. Determination of total and methylmercury compounds in the IAEA human hair intercomparison samples - Experience of the IAEA-MEL

    International Nuclear Information System (INIS)

    Horvat, M.; Liang, L.; Mandic, V.

    1995-01-01

    The programme of this CRP is focused on the analyses of human hair samples. There are only two human hair samples certified for total mercury, and no RMs for methylmercury compounds is available. One of the main objectives of this CRP is to produce, through the IAEA AQCS Programme, a human hair intercomparison material for quality assurance requirements in population monitoring programmes for total and methylmercury exposure. Through the reporting period, MESL has introduced a new method for simultaneous determination of total and methylmercury in biological samples. As the laboratory has close collaboration with the CRP's Reference Laboratory in Ljubljana, Slovenia, it has also been actively involved in the quality assurance component of this CRP. This report represents a summary on the results for total and methylmercury in two intercomparison samples, IAEA-085 and IAEA-086 using newly developed method

  4. Simultaneous Determination of 14 Phenolic Compounds in Grape Canes by HPLC-DAD-UV Using Wavelength Switching Detection

    Directory of Open Access Journals (Sweden)

    Ang Zhang

    2013-11-01

    Full Text Available The paper described a novel chromatographic method for the simultaneous determination of phenolic compounds such as gallic, protocatechuic, vanillic, caffeic, syringic, p-coumaric and salicylic acid, (+-catechin, (‒-epicatechin, rutin, morin, quercetin, coumarin and trans-resveratrol at their maximum absorbance wavelengths (MAW employing reverse-phase high performance liquid chromatography combined with DAD and UV detection via detection wavelength switching. The method was based on MAW acquisition by DAD and quantification by UV. The separation process was performed on a Shim-Pack VP-ODS C18 column (250 mm × 4.6 mm, 5 μm held at 30 °C, utilizing 3.0% acetic acid and acetonitrile as mobile phase at a flow rate of 0.8 mL/min in the gradient elution mode. The method was fully validated in terms of linearity (r2 > 0.9990, 10‒350 mg/L, precision (both intra-day and inter-day RSD < 4.22%, accuracy (97.31%‒104.66%, specificity, robustness (0.59% < RSD < 2.86%, limit of detection and quantification. The switching method significantly improved the sensitivities of most phenolics studied in comparison with the standard constant wavelength detection (280 nm. The proposed method has been successfully applied to the determination of 14 phenolic compounds in 89 varieties of one-year-old Chinese grape one-year-canes. Grape canes contain many phenolics, especially trans-resveratrol, (‒-epicatechin, and (+-catechin.

  5. Determination of bismuth in environmental samples by ICP-MS and basic examination of cell toxicity for their compounds

    International Nuclear Information System (INIS)

    Kobayashi, Jun; Matsukawa, Takehisa; Chiba, Momoko; Yokoyama, Kazuhito; Terada, Hiroshi; Sugiyama, Hideo

    2011-01-01

    We examined both bismuth content levels in some environmental water samples (tapwater, bottled drinking water and slag obtained by sewage disposal) by inductively coupled plasma mass spectrometry (ICP-MS) and cultured cell toxicity of their compounds by the MTT assay. For ICP-MS, the conditions examined were addition of internal standard (IS), apparatus condition, and determination range, etc. When we examined an IS, the advantage was not clear that the ICP-MS response of the IS candidate elements was very variable. However, the sample induction rate into ICP-MS is more changeable at any time. Since the correction of analytical results was enabled by the addition of IS, Tl-203 was selected for IS, and was used in this study. The determination lower limit was 11 ppt by using 10 ppb Tl. Bi was detected in a few environmental water samples at 20.4 ppt - 6.8 ppb (0.07-6.83 μg/g original slags), but Bi concentrations of most samples were lower than the determination limit. On the other hand, concerning cell toxicity, the subgallate and free gallic acid affected the lives of cultured cells. Especially, the toxicity of free gallic acid was higher. It has been understood that the toxicity is weakly adjusted by chelating with Bi. (author)

  6. Simple time-saving method for iron determination based on fluorescence quenching of an azaflavanon-3-ol compound.

    Science.gov (United States)

    Başoğlu, Aysel; Tosun, Gonca; Ocak, Miraç; Alp, Hakan; Yaylı, Nurettin; Ocak, Ümmühan

    2015-03-18

    A simple and time-saving spectrofluorometric method developed using an azaflavanon-3-ol compound was used for the determination of iron in various food samples. Nitric acid and hydrogen peroxide were used for digestion of samples in a closed microwave system. The method was validated by analyzing two certified reference materials (CRM-SA-C Sandy Soil C and Mixed Polish Herbs INCT-MPH-2). Measurements were carried out using a modified standard addition method. The standard addition graph was linear until 21.6 mg/L in the determination of iron(III). Detection and quantification limits were 0.81 and 2.4 mg/L, respectively. Satisfactory accuracy was obtained for spinach, dill, mint, purslane, rocket, red lentils, dry beans, and two iron medicinal tablets. High recoveries were found for streamwater samples fortified at three different concentrations. The method is simple, time-saving, cost-effective, and suitable for the determination of the iron content of foods.

  7. Determination of quaternary ammonium compounds by potentiometric titration with an ionic surfactant electrode: single-laboratory validation.

    Science.gov (United States)

    Price, Randi; Wan, Ping

    2010-01-01

    A potentiometric titration for determining the quaternary ammonium compounds (QAC) commonly found in antimicrobial products was validated by a single laboratory. Traditionally, QACs were determined by using a biphasic (chloroform and water) manual titration procedure. Because of safety considerations regarding chloroform, as well as the subjectivity of color indicator-based manual titration determinations, an automatic potentiometric titration procedure was tested with quaternary nitrogen product formulations. By using the Metrohm Titrando system coupled with an ionic surfactant electrode and an Ag/AgCl reference electrode, titrations were performed with various QAC-containing formulation products/matrixes; a standard sodium lauryl sulfate solution was used as the titrant. Results for the products tested are sufficiently reproducible and accurate for the purpose of regulatory product enforcement. The robustness of the method was measured by varying pH levels, as well as by comparing buffered versus unbuffered titration systems. A quantitation range of 1-1000 ppm quaternary nitrogen was established. Eight commercially available antimicrobial products covering a variety of matrixes were assayed; the results obtained were comparable to those obtained by the manual titration method. Recoveries of 94 to 104% were obtained for spiked samples.

  8. Applicability of solid-phase microextraction combined with gas chromatography atomic emission detection (GC-MIP AED) for the determination of butyltin compounds in sediment samples

    Energy Technology Data Exchange (ETDEWEB)

    Carpinteiro, J.; Rodriguez, I.; Cela, R. [Universidad de Santiago de Compostela, Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacion y Analisis Alimentario, Santiago de Compostela 15782 (Spain)

    2004-11-01

    The performance of solid-phase microextraction (SPME) applied to the determination of butyltin compounds in sediment samples is systematically evaluated. Matrix effects and influence of blank signals on the detection limits of the method are studied in detail. The interval of linear response is also evaluated in order to assess the applicability of the method to sediments polluted with butyltin compounds over a large range of concentrations. Advantages and drawbacks of including an SPME step, instead of the classic liquid-liquid extraction of the derivatized analytes, in the determination of butyltin compounds in sediment samples are considered in terms of achieved detection limits and experimental effort. Analytes were extracted from the samples by sonication using glacial acetic acid. An aliquot of the centrifuged extract was placed on a vial where compounds were ethylated and concentrated on a PDMS fiber using the headspace mode. Determinations were carried out using GC-MIP AED. (orig.)

  9. A fast and simple method for quantitative determination of fat-derived medium and low-volatile compounds in cheese

    NARCIS (Netherlands)

    Alewijn, M.; Sliwinski, E.L.; Wouters, J.T.M.

    2003-01-01

    Cheese flavour is a mixture of many (volatile) compounds, mostly formed during ripening. The current method was developed to qualify and quantify fat-derived compounds in cheese. Cheese samples were extracted with acetonitrile, which led to a concentrated solution of potential favour compounds,

  10. Determination of organic compounds in medicinal plants, commercialized in capsulated forms and 'in natura' by wavelength dispersive X-ray fluorescence spectrometry (WDXRF). Determination of quantitative inorganic profiles

    International Nuclear Information System (INIS)

    Ferreira, Manuel Octavio M.; Sato, Ivone Mulako; Salvador, Vera Lucia R.

    2005-01-01

    X-ray fluorescence technique was used to determine major and trace elements for five Brazilian commercial medicinal plants. The bromobutane (Barbatimao), Ginkgo folium (Ginkgo biloba), Echinodorus macrophyllus (Chapeu de couro), Valeriana officinalis (Valeriana), Cordia salicifolia (Porangaba) samples were collected from three to six different commercial suppliers. The species were collected 'in natura' (leaves, flowers, barks and roots) and capsulated forms. The samples were grinded in liquid N 2 atmosphere and double layer pressed pellet were prepared. The elements Na, Mg, P, S, Cl, K, Ca, Mn, Fe, Ni, Cu, Zn, Rb e Sr concentrations were determined by individual calibration curves. The precision and accuracy of method were evaluated by certified reference material, NIST 1547 - Peach Leaves and the Chauvenet, Cochrane, ANOVA and Z-score statistical tests were applied. Each specimen presented a distinct inorganic profile and a great variation in its composition was observed. The inorganic profile will contribute for the elaboration of a quality and security guide to assure the phytotherapics commercialization. Moreover, these profiles could be used as complementary data to active farmaco compounds profiles for specimen's ratification. (author)

  11. Determination of Selected Polycyclic Aromatic Compounds in Particulate Matter Samples with Low Mass Loading: An Approach to Test Method Accuracy

    Directory of Open Access Journals (Sweden)

    Susana García-Alonso

    2017-01-01

    Full Text Available A miniaturized analytical procedure to determine selected polycyclic aromatic compounds (PACs in low mass loadings (<10 mg of particulate matter (PM is evaluated. The proposed method is based on a simple sonication/agitation method using small amounts of solvent for extraction. The use of a reduced sample size of particulate matter is often limiting for allowing the quantification of analytes. This also leads to the need for changing analytical procedures and evaluating its performance. The trueness and precision of the proposed method were tested using ambient air samples. Analytical results from the proposed method were compared with those of pressurized liquid and microwave extractions. Selected PACs (polycyclic aromatic hydrocarbons (PAHs and nitro polycyclic aromatic hydrocarbons (NPAHs were determined by liquid chromatography with fluorescence detection (HPLC/FD. Taking results from pressurized liquid extractions as reference values, recovery rates of sonication/agitation method were over 80% for the most abundant PAHs. Recovery rates of selected NPAHs were lower. Enhanced rates were obtained when methanol was used as a modifier. Intermediate precision was estimated by data comparison from two mathematical approaches: normalized difference data and pooled relative deviations. Intermediate precision was in the range of 10–20%. The effectiveness of the proposed method was evaluated in PM aerosol samples collected with very low mass loadings (<0.2 mg during characterization studies from turbofan engine exhausts.

  12. Optimization and Application of a GC-MS Method for the Determination of Endocrine Disruptor Compounds in Natural Water

    Directory of Open Access Journals (Sweden)

    José Gustavo Ronderos-Lara

    2018-06-01

    Full Text Available Bisphenol A (BPA, 4-nonylphenol (4NP, estradiol (E2, and ethinylestradiol (EE2 are considered as endocrine disruptors or mutagens. These compounds are commonly called endocrine disrupter chemicals (EDCs. BPA and 4NP are widely used as plastic additives, lacquers, resins, or surfactants, while E2 is one of the predominant female sex hormones during the reproductive years, and EE2 is an estrogen derived from estradiol, used in the production of contraceptive pills. All of these can be usually found in wastewater. In Mexico, it is common for water from rivers, lakes, and canyons to be reused for different purposes. Unfortunately, there is little information on the concentration of many of the pollutants present in such bodies of water. To determine the presence of these compounds in samples of wastewater in the Apatlaco River, an accurate and reproducible method was developed by coupling gas chromatography to mass spectrometry (GC-MS. A solid-phase extraction with Chromabond RP-18 cartridges was carried out, and the elution was performed with an acetone/methanol mixture. After isolation, the solvent was removed and a silylation step was carried out using N,O-bis(trimethylsilyltrifluoroacetamide (BSTFA. Recoveries for spiked samples were between 71.8% and 111.0%. The instrumental limits of detection (IDL ranged between 24.7 and 37.0 ng mL−1. In total, 16 samples were taken in 2015 at the microbasin of the Apatlaco River, located in the state of Morelos. The maximum concentrations found were 4NP (85.5 ng mL−1, BPA (174.6 ng mL−1, E2 103.6 (ng mL−1, and EE2 (624.3 ng mL−1.

  13. Micelle assisted thin-film solid phase microextraction: a new approach for determination of quaternary ammonium compounds in environmental samples.

    Science.gov (United States)

    Boyacı, Ezel; Pawliszyn, Janusz

    2014-09-16

    Determination of quaternary ammonium compounds (QACs) often is considered to be a challenging undertaking owing to secondary interactions of the analytes' permanently charged quaternary ammonium head or hydrophobic tail with the utilized labware. Here, for the first time, a micelle assisted thin-film solid phase microextraction (TF-SPME) using a zwitterionic detergent 3-[(3-cholamidopropyl)dimethylammonio]-1-propanesulfonate (CHAPS) as a matrix modifier is introduced as a novel approach for in-laboratory sample preparation of the challenging compounds. The proposed micelle assisted TF-SPME method offers suppression/enhancement free electrospray ionization of analytes in mass spectrometric detection, minimal interaction of the micelles with the TF-SPME coating, and chromatographic stationary phase and analysis free of secondary interactions. Moreover, it was found that the matrix modifier has multiple functions; when its concentration is found below the critical micelle concentration (CMC), the matrix modifier primarily acts as a surface deactivator; above its CMC, it acts as a stabilizer for QACs. Additionally, shorter equilibrium extraction times in the presence of the modifier demonstrated that micelles also assist in the transfer of analytes from the bulk of the sample to the surface of the coating. The developed micelle assisted TF-SPME protocol using the 96-blade system requires only 30 min of extraction and 15 min of desorption. Together with a conditioning step (15 min), the entire method is 60 min; considering the advantage of using the 96-blade system, if all the blades in the brush are used, the sample preparation time per sample is 0.63 min. Moreover, the recoveries for all analytes with the developed method were found to range within 80.2-97.3%; as such, this method can be considered an open bed solid phase extraction. The proposed method was successfully validated using real samples.

  14. Quantitative determination of solid-state forms of a pharmaceutical development compound in drug substance and tablets.

    Science.gov (United States)

    Xie, Yong; Tao, Wenle; Morrison, Henry; Chiu, Rick; Jona, Janan; Fang, Jan; Cauchon, Nina

    2008-10-01

    Common analytical techniques including Raman, NIR, and XRD were evaluated for quantitative determination of three solid-state forms (amorphous, Form B and Form C) of a development compound. Raman spectroscopy was selected as the primary analytical technique with sufficient sensitivity to monitor and quantify the neat drug substance alone and in the drug product. A reliable multivariate curve resolution (MCR) method based on the second derivative Raman measurements of the three pure physical forms was developed and validated with 3.5% root mean square error of prediction (RMSEP) for Form B, which was selected as the preferred form for further development. A partial least squares (PLS) algorithm was also used for the multivariate calibration of both the NIR and Raman measurements. The long-term stability of Form B as a neat active pharmaceutical ingredient (API) and in a tablet formulation was quantitatively monitored under various stress conditions of temperature and moisture. Moisture, temperature, excipients and compression were found to have significant effects on the phase transition behavior of Form B.

  15. Simultaneous Determination of 11 Compounds in Gualou Guizhi Granule and Pharmacokinetics Study by UPLC-MS/MS

    Directory of Open Access Journals (Sweden)

    Chengtao Sun

    2017-01-01

    Full Text Available A rapid and sensitive ultrafast performance liquid chromatography-tandem mass spectrometry method (UPLC-MS/MS was developed for the simultaneous determination of 11 compounds in Gualou Guizhi Granule (GLGZG, including liquiritin, isoliquiritin, liquirtin apioside, isoliquiritin apioside, liquiritigenin, isoliquiritigenin, glycyrrhizic acid, glycyrrhetinic acid, paeoniflorin, albiflorin, and paeoniflorin sulfonate in rat plasma. UPLC-MS/MS assay with negative ion mode was performed on a Waters CORTECS C18 (2.1 × 100 mm, 1.6 μm with the mobile phase consisting of 0.1% aqueous formic acid (A and acetonitrile (B in gradient elution at a flow rate of 0.25 mL·min−1. The method was linear for all analytes within the detection range (r≥0.9597. The inter- and intraday precision (RSD were 2.21–6.41% and 1.67–6.18%; the inter- and intraday accuracy (recover were 92.48–114.03% and 90.23–112.04%. And the recovery rate ranged from 81.30% to 108.22%. The matrix effect values obtained for analytes ranged from 88.91% to 113.32%. This validated method was successfully applied to a pharmacokinetics study in rats after oral administration of GLGZG.

  16. Role of management strategies and environmental factors in determining the emissions of biogenic volatile organic compounds from urban greenspaces.

    Science.gov (United States)

    Ren, Yuan; Ge, Ying; Gu, Baojing; Min, Yong; Tani, Akira; Chang, Jie

    2014-06-03

    Biogenic volatile organic compound (BVOC) emissions from urban greenspace have recently become a global concern. To identify key factors affecting the dynamics of urban BVOC emissions, we built an estimation model and utilized the city of Hangzhou in southeastern China as an example. A series of single-factor scenarios were first developed, and then nine multifactor scenarios using a combination of different single-factor scenarios were built to quantify the effects of environmental changes and urban management strategies on urban BVOC emissions. Results of our model simulations showed that (1) annual total BVOC emissions from the metropolitan area of Hangzhou were 4.7×10(8) g of C in 2010 and were predicted to be 1.2-3.2 Gg of C (1 Gg=10(9) g) in our various scenarios in 2050, (2) urban management played a more important role in determining future urban BVOC emissions than environmental changes, and (3) a high ecosystem service value (e.g., lowest BVOC/leaf mass ratio) could be achieved through positive coping in confronting environmental changes and adopting proactive urban management strategies on a local scale, that is, to moderately increase tree density while restricting excessive greenspace expansion and optimizing the species composition of existing and newly planted trees.

  17. Determination of tetrachloroethylene and other volatile halogenated organic compounds in oil wastes by headspace SPME GC-MS

    Energy Technology Data Exchange (ETDEWEB)

    Fabbri, D.; Bezzi, R.; Torri, C.; Galletti, P.; Tagliavini, E. [Bologna Univ., Ravenna (Italy). Lab. of Chemistry, C.I.R.S.A

    2007-09-15

    Oil wastes and slops are complex mixtures of hydrocarbons, which may contain a variety of contaminants including tetrachloroethylene (perchloroethylene, PCE) and other volatile halogenated organic compounds (VHOCs). The analytical determination of PCE at trace levels in petroleum-derived matrices is difficult to carry out in the presence of large amounts of hydrocarbon matrix components. In the following study, we demonstrate that headspace solid-phase microextraction (HS-SPME) combined with GC-MS analysis can be applied for the rapid measurement of PCE concentration in oil samples. The HS-SPME method was developed using liquid paraffin as matrix matching reference material for external and internal calibration and optimisation of experimental parameters. The limit of quantitation was 0.05 mg kg{sup -1}, and linearity was established up to 25 mg kg{sup -1}. The HS-SPME method was extended to several VHOCs, including trichloroethylene (TCE) in different matrices and was applied to the quantitative analysis of PCE and TCE in real samples.

  18. Marine mammal blubber reference and control materials for use in the determination of halogenated organic compounds and fatty acids

    Energy Technology Data Exchange (ETDEWEB)

    Kucklick, John R.; Pugh, Rebecca S.; Becker, Paul R. [Hollings Marine Laboratory, National Institute of Standards and Technology (NIST), Charleston, SC (United States); Schantz, Michele M.; Porter, Barbara J.; Poster, Dianne L.; Leigh, Stefan; Wise, Stephen A. [NIST, Analytical Chemistry Division, Gaithersburg, MD (United States); Rowles, Teri K. [National Marine Fisheries Service, National Oceanic and Atmospheric Administration, Silver Spring, MD (United States)

    2010-05-15

    The National Institute of Standards and Technology (NIST) has a diverse collection of control materials derived from marine mammal blubber, fat, and serum. Standard Reference Material (SRM) 1945 Organics in Whale Blubber was recertified for polychlorinated biphenyl (PCB) congeners, organochlorine pesticides, and polybrominated diphenyl ether (PBDE) congeners. SRM 1945 has also been assigned mass fraction values for compounds not frequently determined in marine samples including toxaphene congeners, coplanar PCBs, and methoxylated PBDE congeners which are natural products. NIST also has assigned mass fraction values, as a result of interlaboratory comparison exercises, for PCB congeners, organochlorine pesticides, PBDE congeners, and fatty acids in six homogenate materials produced from marine mammal blubber or serum. The materials are available from NIST upon request; however, the supply is very limited for some of the materials. The materials include those obtained from pilot whale blubber (Homogenates III and IV), Blainville's beaked whale blubber (Homogenate VII), polar bear fat (Homogenate VI), and California sea lion serum (Marine Mammal Control Material-1 Serum) and blubber (Homogenate V). (orig.)

  19. Fast and effective low-temperature freezing extraction technique to determine organotin compounds in edible vegetable oil.

    Science.gov (United States)

    Liu, Yingxia; Ma, Yaqian; Wan, Yiqun; Guo, Lan; Wan, Xiaofen

    2016-06-01

    Most organotin compounds that have been widely used in food packaging materials and production process show serious toxicity effects to human health. In this study, a simple and low-cost method based on high-performance liquid chromatography with inductively coupled plasma mass spectrometry for the simultaneous determination of four organotins in edible vegetable oil samples was developed. Four organotins including dibutyltin dichloride, tributyltin chloride, diphenyltin dichloride, and triphenyltin chloride were simultaneously extracted with methanol using the low-temperature precipitation process. After being concentrated, the extracts were purified by matrix solid-phase dispersion using graphitized carbon black. The experimental parameters such as extraction solvent and clean-up material were optimized. To evaluate the accuracy of the new method, the recoveries were investigated. In addition, a liquid chromatography with tandem mass spectrometry method was also proposed for comparison. The procedures of extracting and purifying samples for the analysis were simple and easy to perform batch operations, also showed good efficiency with lower relative standard deviation. The limits of detection of the four organotins were 0.28-0.59 μg/L, and the limits of quantification of the four organotins were 0.93-1.8 μg/L, respectively. The proposed method was successfully applied to the simultaneous analysis of the four organotins in edible vegetable oil. Some analytes were detected at the level of 2.5-28.8 μg/kg. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Determination of sugar compounds in olive plant extracts by anion-exchange chromatography with pulsed amperometric detection.

    Science.gov (United States)

    Cataldi, T R; Margiotta, G; Iasi, L; Di Chio, B; Xiloyannis, C; Bufo, S A

    2000-08-15

    We describe a chromatographic method that uses isocratic elution and pulsed amperometric detection to determine soluble carbohydrates in plant tissues. Such a method provides a rapid and convenient means to obtain a complete profile of the sugar components of leaves and roots from olive (Olea europaea L. cv. Coratina) plants. A simple purification of plant extracts using pure water was developed, which is far less time-consuming and retains a high level of accuracy. Excellent separation of myo-inositol, galactinol, mannitol, galactose, glucose, fructose, sucrose, raffinose, and stachyose was achieved with an anion-exchange column and 12 mM NaOH spiked with 1 mM barium acetate as an eluent. At a flow rate of 1.0 mL/min, the time of analysis was less than 25 min, and repeatability of the method on the order of 2.2% as RSD or better for retention times and lower than 5.2% for peak areas. Recoveries approximated 100% (range 97.2-104.5%), and the method provided good precision with a coefficient of variation which ranged between 0.9 and 3.3%. Among identified carbohydrates extracted from leaves and roots of olive plants, glucose and mannitol were major compounds. Their molar ratio was estimated to be 1.2+/-0.1 and 2.2+/-0.3 for olive leaves and roots, respectively. The occurrence of soluble galactinol in plant tissues was also validated.

  1. Polymeric ionic liquid coatings versus commercial solid-phase microextraction coatings for the determination of volatile compounds in cheeses.

    Science.gov (United States)

    Trujillo-Rodríguez, María J; Yu, Honglian; Cole, William T S; Ho, Tien D; Pino, Verónica; Anderson, Jared L; Afonso, Ana M

    2014-04-01

    The extraction performance of four polymeric ionic liquid (PIL)-based solid-phase microextraction (SPME) coatings has been studied and compared to that of commercial SPME coatings for the extraction of 16 volatile compounds in cheeses. The analytes include 2 free fatty acids, 2 aldehydes, 2 ketones and 10 phenols and were determined by headspace (HS)-SPME coupled to gas chromatography (GC) with flame-ionization detection (FID). The PIL-based coatings produced by UV co-polymerization were more efficient than PIL-based coatings produced by thermal AIBN polymerization. Partition coefficients of analytes between the sample and the coating (Kfs) were estimated for all PIL-based coatings and the commercial SPME fiber showing the best performance among the commercial fibers tested: carboxen-polydimethylsyloxane (CAR-PDMS). For the PIL-based fibers, the highest K(fs) value (1.96 ± 0.03) was obtained for eugenol. The normalized calibration slope, which takes into account the SPME coating thickness, was also used as a simpler approximate tool to compare the nature of the coating within the determinations, with results entirely comparable to those obtained with estimated K(fs) values. The PIL-based materials obtained by UV co-polymerization containing the 1-vinyl-3-hexylimidazolium chloride IL monomer and 1,12-di(3-vinylimiazolium)dodecane dibromide IL crosslinker exhibited the best performance in the extraction of the select analytes from cheeses. Despite a coating thickness of only 7 µm, this copolymeric sorbent coating was capable of quantitating analytes in HS-SPME in a 30 to 2000 µg L(-1) concentration range, with correlation coefficient (R) values higher than 0.9938, inter-day precision values (as relative standard deviation in %) varying from 6.1 to 20%, and detection limits down to 1.6 µg L(-1). Copyright © 2013 Elsevier B.V. All rights reserved.

  2. Multicommuted flow injection method for fast photometric determination of phenolic compounds in commercial virgin olive oil samples.

    Science.gov (United States)

    Lara-Ortega, Felipe J; Sainz-Gonzalo, Francisco J; Gilbert-López, Bienvenida; García-Reyes, Juan F; Molina-Díaz, Antonio

    2016-01-15

    A multicommuted flow injection method has been developed for the determination of phenolic species in virgin olive oil samples. The method is based on the inhibitory effect of antioxidants on a stable and colored radical cation formation from the colorless compound N,N-dimethyl-p-phenylenediamine (DMPD(•+)) in acidic medium in the presence of Fe(III) as oxidant. The signal inhibition by phenolic species and other antioxidants is proportional to their concentration in the olive oil sample. Absorbance was recorded at 515nm by means of a modular fiber optic spectrometer. Oleuropein was used as the standard for phenols determination and 6-hydroxy-2,5,7,8-tetramethylchroman-2-carboxylic acid (trolox) was the reference standard used for total antioxidant content calculation. Linear response was observed within the range of 250-1000mg/kg oleuropein, which was in accordance with phenolic contents observed in commercial extra virgin olive oil in the present study. Fast and low-volume liquid-liquid extraction of the samples using 60% MeOH was made previous to their insertion in the flow multicommuted system. The five three-way solenoid valves used for multicommuted liquid handling were controlled by a homemade electronic interface and Java-written software. The proposed approach was applied to different commercial extra virgin olive oil samples and the results were consistent with those obtained by the Folin Ciocalteu (FC) method. Total time for the sample preparation and the analysis required in the present approach can be drastically reduced: the throughput of the present analysis is 8 samples/h in contrast to 1sample/h of the conventional FC method. The present method is easy to implement in routine analysis and can be regarded as a feasible alternative to FC method. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. Determination of endocrine-disrupting compounds in drinking waters by fast liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Magi, Emanuele; Scapolla, Carlo; Di Carro, Marina; Liscio, Camilla

    2010-09-01

    Growing attention has been recently paid to safety of food and drinking water, making necessary the adoption of policies for water sources protection and the development of sensitive and rapid analytical methods to identify micropollutants. Endocrine-disrupting compounds (EDCs) have emerged as a major issue as they alter the functioning of the endocrine system. Since ingestion of EDCs via food is considered the major exposure route, there is a growing interest in understanding EDC fate during drinking water treatment and in monitoring potential contamination of surface waters and groundwaters. In this work, a fast liquid chromatography-electrospray ionization-tandem mass spectrometry method was developed for the determination of 4-n-nonylphenol (NP), bisphenol A (BPA), estrone (E1), 17β-estradiol (E2) and 17α-ethinylestradiol (EE2) in drinking waters. In the literature analytical articles seldom provide details regarding fragmentation pathways. In this paper spectra of the five EDCs in negative ESI were interpreted with the support of accurate mass spectra acquired by a quadrupole time-of-flight instrument; fragmentation pathways were also proposed. The chromatographic separation of EDCs was optimized on a Pinnacle DB Biphenylic column with a water-acetonitrile gradient. Quantitative analysis was performed in multiple reaction monitoring (MRM) mode using bisphenol A-d(16) (BPA-d(16)) as internal standard; calibration curves showed good correlation coefficients (0.9989-0.9997). All figures of merit of the method were satisfactory; limits of detection were in the range 0.2-0.4 ng/ml. The method was applied to the determination of the analytes in waters sampled by polar organic chemical integrative samplers in a drinking water treatment plant. Rather low concentration of BPA, NP and E1 were measured in the inlet, while none of the considered EDCs was detected in the outlet. 2010 John Wiley & Sons, Ltd.

  4. Chemical structure of bismuth compounds determines their gastric ulcer healing efficacy and anti-Helicobacter pylori activity.

    Science.gov (United States)

    Sandha, G S; LeBlanc, R; Van Zanten, S J; Sitland, T D; Agocs, L; Burford, N; Best, L; Mahoney, D; Hoffman, P; Leddin, D J

    1998-12-01

    The recognition of the role of Helicobacter pylori in the pathogenesis of peptic ulcer disease has led to renewed interest in bismuth pharmacology since bismuth compounds have both anti-Helicobacter pylori and ulcer healing properties. The precise chemical structure of current bismuth compounds is not known. This has hindered the development of new and potentially more efficacious formulations. We have created two new compounds, 2-chloro-1,3-dithia-2-bismolane (CDTB) and 1,2-[bis(1,3-dithia-2-bismolane)thio]ethane (BTBT), with known structure. In a rat model of gastric ulceration, BTBT was comparable to, and CDTB was significantly less effective than colloidal bismuth subcitrate in healing cryoprobe-induced ulcers. However, both BTBT and CDTB inhibited H. pylori growth in vitro at concentrations <1/10 that of colloidal bismuth subcitrate. The effects on ulcer healing are not mediated by suppression of acid secretion, pepsin inhibition, or prostaglandin production. Since all treated animals received the same amount of elemental bismuth, it appears that the efficacy of bismuth compounds varies with compound structure and is not simply dependent on the delivery of bismuth ion. Because the structure of the novel compounds is known, our understanding of the relationship of bismuth compound structure and to biologic activity will increase. In the future it may be possible to design other novel bismuth compounds with more potent anti-H. pylori and ulcer healing effects.

  5. Modified solution calorimetry approach for determination of vaporization and sublimation enthalpies of branched-chain aliphatic and alkyl aromatic compounds at T = 298.15 K

    International Nuclear Information System (INIS)

    Varfolomeev, Mikhail A.; Novikov, Vladimir B.; Nagrimanov, Ruslan N.; Solomonov, Boris N.

    2015-01-01

    Highlights: • Solution enthalpies of 18 branching-chain alkyl aromatic and aliphatic compounds in cyclohexane were measured. • Group contributions to the enthalpy of solvation due to branching and substitution in carbon chain were evaluated. • Modified solution calorimetry based approach for determination of vaporization/sublimation enthalpies was proposed. • This approach provides vaporization/sublimation enthalpies directly at T = 298.15 K. • Vaporization/sublimation enthalpies of 35 branched-chain alkyl aromatic and aliphatic compounds were determined. - Abstract: The enthalpies of solution, solvation and vaporization/sublimation are interrelated values combined in the simplest thermodynamic circle. Hence, experimental determination of vaporization/sublimation enthalpy can be substituted by experimentally simpler determination of solution enthalpy when solvation enthalpy is known. Previously it was found that solvation enthalpies of a wide range of unbranched aliphatic and aromatic solutes in saturated hydrocarbons are in good linear correlation with their molar refraction values. This allows to estimate the vaporization/sublimation enthalpy of any unbranched organic compound from its solution enthalpy in saturated hydrocarbon and molar refraction. In the present work this approach was modified for determination of vaporization/sublimation enthalpy of branched-chain alkyl aromatic and aliphatic compounds. Group contributions to the enthalpy of solvation due to the branching of carbon chain were evaluated. Enthalpies of solution at infinite dilution of 18 branched-chain aliphatic and alkyl aromatic compounds were measured at T = 298.15 K. Vaporization/sublimation enthalpies for 35 branched aliphatic and alkyl aromatic compounds were determined by using modified solution calorimetry approach. These values are in good agreement with available literature data on vaporization/sublimation enthalpies obtained by conventional methods.

  6. Gas chromatographic-mass spectrometric determination of hydrophilic compounds in environmental water by solid-phase extraction with activated carbon fiber felt.

    Science.gov (United States)

    Kawata, K; Ibaraki, T; Tanabe, A; Yagoh, H; Shinoda, A; Suzuki, H; Yasuhara, A

    2001-03-09

    Simple gas chromatographic-mass spectrometric determination of hydrophilic organic compounds in environmental water was developed. A cartridge containing activated carbon fiber felt was made by way of trial and was evaluated for solid-phase extraction of the compounds in water. The hydrophilic compounds investigated were acrylamide, N,N-dimethylacetamide, N,N-dimethylformamide, 1,4-dioxane, furfural, furfuryl alcohol, N-nitrosodiethylamine and N-nitrosodimethylamine. Overall recoveries were good (80-100%) from groundwater and river water. The relative standard deviations ranged from 4.5 to 16% for the target compounds. The minimum detectable concentrations were 0.02 to 0.03 microg/l. This method was successfully applied to several river water samples.

  7. Determination of free amino compounds in betalainic fruits and vegetables by gas chromatography with flame ionization and mass spectrometric detection.

    Science.gov (United States)

    Kugler, Florian; Graneis, Stephan; Schreiter, Pat P-Y; Stintzing, Florian C; Carle, Reinhold

    2006-06-14

    Amino acids and amines are the precursors of betalains. Therefore, the profiles of free amino compounds in juices obtained from cactus pears [Opuntia ficus-indica (L.) Mill. cv. Bianca, cv. Gialla, and cv. Rossa], pitaya fruits [Selenicereus megalanthus (K. Schumann ex Vaupel) Moran, Hylocereus polyrhizus (Weber) Britton & Rose, and Hylocereus undatus (Haworth) Britton & Rose], and in extracts from differently colored Swiss chard [Beta vulgaris L. ssp. cicla (L.) Alef. cv. Bright Lights] petioles and red and yellow beets (B. vulgaris L. ssp. vulgaris var. conditiva Alef. cv. Burpee's Golden) were investigated for the first time. Amino compounds were derivatized with propyl chloroformate. While gas chromatography (GC) with mass spectrometry was used for peak assignment, GC flame ionization detection was applied for quantification of individual compounds. Whereas proline was the major free amino compound of cactus pear and pitaya fruit juices, glutamine dominated in Swiss chard stems and beets, respectively. Interestingly, extremely high concentrations of dopamine were detected in Swiss chard stems and beets. Furthermore, the cleavage of betaxanthins caused by derivatization in alkaline reaction solutions is demonstrated for the first time. Amino acids and amines thus released might increase the actual free amino compound contents of the respective sample. To evaluate the contribution of betaxanthin cleavage to total amino acid and amine concentration, isolated betaxanthins were derivatized according to the "EZ:faast" method prior to quantification of the respective amino compounds released. On a molar basis, betaxanthin contribution to overall amino compound contents was always below 6.4%.

  8. observed by high pressure NMR and NQR

    Indian Academy of Sciences (India)

    Akogun, Hyogo 678-1297, Japan. ∗. Email: kohara@sci.himeji tech.ac.jp. Abstract. NMR and NQR studies on two interesting systems (URu2Si2, CeTIn5) were performed under high pressure. (1) URu2Si2: In the pressure range 3.0 to 8.3 kbar, we have observed new 29Si. NMR signals arising from the antiferromagnetic ...

  9. Peptidylation for the determination of low-molecular-weight compounds by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry.

    Science.gov (United States)

    Tang, Feng; Cen, Si-Ying; He, Huan; Liu, Yi; Yuan, Bi-Feng; Feng, Yu-Qi

    2016-05-23

    Determination of low-molecular-weight compounds by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) has been a great challenge in the analytical research field. Here we developed a universal peptide-based derivatization (peptidylation) strategy for the sensitive analysis of low-molecular-weight compounds by MALDI-TOF-MS. Upon peptidylation, the molecular weights of target analytes increase, thus avoiding serious matrix ion interference in the low-molecular-weight region in MALDI-TOF-MS. Since peptides typically exhibit good signal response during MALDI-TOF-MS analysis, peptidylation endows high detection sensitivities of low-molecular-weight analytes. As a proof-of-concept, we analyzed low-molecular-weight compounds of aldehydes and thiols by the developed peptidylation strategy. Our results showed that aldehydes and thiols can be readily determined upon peptidylation, thus realizing the sensitive and efficient determination of low-molecular-weight compounds by MALDI-TOF-MS. Moreover, target analytes also can be unambiguously detected in biological samples using the peptidylation strategy. The established peptidylation strategy is a universal strategy and can be extended to the sensitive analysis of various low-molecular-weight compounds by MALDI-TOF-MS, which may be potentially used in areas such as metabolomics.

  10. Organolanthanoid compounds

    International Nuclear Information System (INIS)

    Schumann, H.

    1984-01-01

    Up to little more than a decade ago organolanthanoid compounds were still a curiosity. Apart from the description of an isolated number of cyclopentadienyl and indenyl derivatives, very few significant contributions had been made to this interesting sector of organometallic chemistry. However, subsequent systematic studies using modern preparative and analytical techniques, together with X-ray single crystal structure determinations, enabled the isolation and characterization of a large number of very interesting homoleptic and heteroleptic compounds in which the lanthanoid is bound to hydrogen, to substituted or unsubstituted cyclopentadienyl groups, to allyl or alkynyl groups, or even to phosphorus ylides, trimethylsilyl, and carbonylmetal groups. These compounds, which are all extremely sensitive to oxygen and water, open up new possibilities in the field of catalysis and have great potential in organic synthesis - as recent studies with pentamethylcyclopentadienyl derivatives, organolanthanoid(II) compounds, and hexamethyllanthanoid complexes have already shown. (orig.) [de

  11. Determination of some volatile compounds in alcoholic beverage by headspace solid-phase microextraction gas chromatography - mass spectrometry

    Science.gov (United States)

    Schmutzer, G.; Avram, V.; Feher, I.; David, L.; Moldovan, Z.

    2012-02-01

    The volatile composition of alcoholic beverage was studied by headspace solid-phase microextraction (HSSPME) method and gas chromatography - mass spectrometry (GC-MS). Some volatile compounds, such as alcohols, esters, terpenes and other are mainly responsible for the flavor of fortified wines and their amounts specify the quality of the alcoholic beverages. From this perspective it is interesting to develop a rapid, selective and sensitive analytical method suitable for simultaneous quantification of the main molecules being responsible for the organoleptic characteristic of alcoholic beverages. Vermouth fortified drink was analyzed in order to characterize the volatile profile. Using the HS-SPME/GC-MS a number of twenty-six volatile compounds from a commercial market alcoholic beverage were identified. The most abundant compounds were m-thymol, o-thymol and eugenol, alongside of the ethyl ester compounds.

  12. The determination of the crystal structures of some uranium compounds by means of x-ray and neutron diffraction

    International Nuclear Information System (INIS)

    Adrian, H.W.W.

    1977-10-01

    In industrial uranium processing or reprocessing procedures, aqueous uranyl nitrate solutions are an intermediate product. The compounds, whose structures are reported, might prove valuable as alternative crystallization products to existing methods of extracting the uranium from solution. The compounds are obtained by the addition of hydroxylammonium to the uranyl nitrate solution and are of the general formula UO 2 (NH 2 0) 2 .xH 2 0, where x can take the values zero, two, three and four. In addition a compound of the formula UO 2 (NH 2 0) 2 .2(NH 2 CH).2H 2 0 was obtained. The UO 2 (NH 2 0) compound crystallized in a monoclinic crystal form. Crystals large enough for neutron diffraction were not obtained. The structure of the UO 2 (NH 2 0) 2 .2H 2 0 could not be solved because only disordered crystalline material was available. The structure of UO 2 (NH 2 0) 2 .3H 2 0 was solved by means of room- and low-temperature neutron diffraction. The unit cell is orthorhombic. The structure of α-UO 2 (NH 2 0) 2 .4H 2 0 was investigated by means of room-temperature x-ray and room- and low-temperature neutron diffraction. The unit cell is triclinic. This compound strongly resembles the trihydrate. The UO 2 (NH 2 0) 2 .2(NH 2 0H).2H 2 0 compound gave crystals large enough for single crystal x-ray but not neutron diffraction. The unit cell is orthorhombic. The characteristic powder patterns (indexed except for the dihydrate compound) of the above compounds are reported [af

  13. Neutron diffraction determination of atomic mean-square displacements in cubic compounds of Ni-Al and Ni-Al-Cu systems

    International Nuclear Information System (INIS)

    Khidirov, I.; Mukhtarova, N.N.

    2002-01-01

    The atomic mean-square displacements (AMSD) are some of important characteristics of the solid and can be the main information for determination of a number of other characteristics of substances. In the work AMSD is determined for a number of cubic compounds of Ni-Al, Ni-Al-Cu systems immediately from intensities of neutron diffraction maxima. It is shown by the offered method that in all NiAl x and NiAlCu x compounds with the CsCl - type structure AMSD are near each other and they are practically constant. Therefore it is possible to assume that within the homogeneity region of these compounds the interatomic bond forces are changed insignificantly

  14. Determination of Wastewater Compounds in Sediment and Soil by Pressurized Solvent Extraction, Solid-Phase Extraction, and Capillary-Column Gas Chromatography/Mass Spectrometry

    Science.gov (United States)

    Burkhardt, Mark R.; Zaugg, Steven D.; Smith, Steven G.; ReVello, Rhiannon C.

    2006-01-01

    A method for the determination of 61 compounds in environmental sediment and soil samples is described. The method was developed in response to increasing concern over the effects of endocrine-disrupting chemicals in wastewater and wastewater-impacted sediment on aquatic organisms. This method also may be used to evaluate the effects of combined sanitary and storm-sewer overflow on the water and sediment quality of urban streams. Method development focused on the determination of compounds that were chosen on the basis of their endocrine-disrupting potential or toxicity. These compounds include the alkylphenol ethoxylate nonionic surfactants and their degradates, food additives, fragrances, antioxidants, flame retardants, plasticizers, industrial solvents, disinfectants, fecal sterols, polycyclic aromatic hydrocarbons, and high-use domestic pesticides. Sediment and soil samples are extracted using a pressurized solvent extraction system. The compounds of interest are extracted from interfering matrix components by high-pressure water/isopropyl alcohol extraction. The compounds were isolated using disposable solid-phase extraction (SPE) cartridges containing chemically modified polystyrene-divinylbenzene resin. The cartridges were dried with nitrogen gas, and then sorbed compounds were eluted with methylene chloride (80 percent)-diethyl ether (20 percent) through Florisil/sodium sulfate SPE cartridge, and then determined by capillary-column gas chromatography/mass spectrometry. Recoveries in reagent-sand samples fortified at 4 to 72 micrograms averaged 76 percent ?13 percent relative standard deviation for all method compounds. Initial method reporting levels for single-component compounds ranged from 50 to 500 micrograms per kilogram. The concentrations of 20 out of 61 compounds initially will be reported as estimated with the 'E' remark code for one of three reasons: (1) unacceptably low-biased recovery (less than 60 percent) or highly variable method performance

  15. Trace-level determination of polar flavour compounds in butter by solid-phase extraction and gas chromatography-mass spectrometry.

    NARCIS (Netherlands)

    Adahchour, M.; Vreuls, J.J.; van der Heijden, A.; Brinkman, U.A.T.

    1999-01-01

    Volatile compounds are responsible for the aromas of butter. A simple technique for the determination of these components is described which is based on solid-phase extraction (SPE) after melting of the butter and separation of the aqueous phase from the fat. Volatile flavours present in the water

  16. THE DETERMINATION OF NON-PESTICIDAL AND PESTICIDAL ORGANOTIN COMPOUNDS IN WATER BY GAS CHROMATOGRAPHY WITH [PULSED] FLAME PHOTOMETRIC DETECTION (GS/PFPD): THE EFFECTS OF "MASS" DISCRIMINATION

    Science.gov (United States)

    Capillary gas chromatography with GC/PFPD was used in the development of analytical methodology for determining both non-pesticidal and pesticidal organotin compounds in drinking water and other aqueous matrices. The method involves aqueous ethylation of organotin analytes with ...

  17. The effect of surfactant on headspace single drop microextraction for the determination of some volatile aroma compounds in citronella grass and lemongrass leaves by gas chromatography

    Science.gov (United States)

    A rapid method for the determination of some volatile aromatic compounds (VACs), including citronellal, citronellol, neral, geranial, geraniol, and eugenol in citronella grass and lemongrass leaves, was developed using surfactant as a surface tension modifier while performing headspace single drop m...

  18. Evaluation of a Silicone Membrane as an Alternative to Human Skin for Determining Skin Permeation Parameters of Chemical Compounds.

    Science.gov (United States)

    Uchida, Takashi; Yakumaru, Masafumi; Nishioka, Keisuke; Higashi, Yoshihiro; Sano, Tomohiko; Todo, Hiroaki; Sugibayashi, Kenji

    2016-01-01

    We evaluated the effectiveness of a silicone membrane as an alternative to human skin using the skin permeation parameters of chemical compounds. An in vitro permeation study using 15 model compounds was conducted, and permeation parameters comprising permeability coefficient (P), diffusion parameter (DL(-2)), and partition parameter (KL) were calculated from each permeation profile. Significant correlations were obtained in log P, log DL(-2), and log KL values between the silicone membrane and human skin. DL(-2) values of model compounds, except flurbiprofen, in the silicone membrane were independent of the lipophilicity of the model compounds and were 100-fold higher than those in human skin. For antipyrine and caffeine, which are hydrophilic, KL values in the silicone membrane were 100-fold lower than those in human skin, and P values, calculated as the product of a DL(-2) and KL, were similar. For lipophilic compounds, such as n-butyl paraben and flurbiprofen, KL values for silicone were similar to or 10-fold higher than those in human skin, and P values for silicone were 100-fold higher than those in human skin. Furthermore, for amphiphilic compounds with log Ko/w values from 0.5 to 3.5, KL values in the silicone membrane were 10-fold lower than those in human skin, and P values for silicone were 10-fold higher than those in human skin. The silicone membrane was useful as a human skin alternative in an in vitro skin permeation study. However, depending on the lipophilicity of the model compounds, some parameters may be over- or underestimated.

  19. Determination of organotin compounds by headspace solid-phase microextraction-gas chromatography-pulsed flame-photometric detection (HS-SPME-GC-PFPD)

    Energy Technology Data Exchange (ETDEWEB)

    Bravo, Manuel [Universite de Pau et des Pays de L' Adour, Laboratoire de Chimie Analytique, LCABIE, UMR CNRS 5034, Pau (France); Pontificia Universidad Catolica de Valparaiso, Laboratorio de Quimica Analitica y Ambiental, Instituto de Quimica, Valparaiso (Chile); Lespes, Gaetane; Gautier, Martine Potin [Pontificia Universidad Catolica de Valparaiso, Laboratorio de Quimica Analitica y Ambiental, Instituto de Quimica, Valparaiso (Chile); Gregori, Ida de; Pinochet, Hugo [Universite de Pau et des Pays de L' Adour, Laboratoire de Chimie Analytique, LCABIE, UMR CNRS 5034, Pau (France)

    2005-12-01

    A method based on Headspace solid-phase microextraction (HS-SPME, with a 100 {mu}m PDMS-fiber) in combination with gas-chromatography and pulsed flame-photometric detection (GC-PFPD) has been investigated for simultaneous determination of eight organotin compounds. Monobutyltin (MBT), dibutyltin (DBT), tributyltin (TBT), monophenyltin (MPhT), and the semi-volatile diphenyltin (DPhT), triphenyltin (TPhT), monooctyltin (MOcT), and dioctyltin (DOcT) were determined after derivatization with sodium tetraethylborate. The conditions used for the extraction and preconcentration step were optimised by experimental design methodology. Tripropyltin (TPrT) and diheptyltin (DHepT) were used as internal standards for quantification of volatile and semi-volatile organotin compounds, respectively. The analytical precision (RSD) for ten successive injections of a standard mixture containing all the organic tin compounds ranged between 2 and 11%. The limits of detection for all the organotin compounds were sub ng (Sn) L{sup -1} in water and close to ng (Sn) kg{sup -1} in sediments. The accuracy of the method was evaluated by analysis of two certified reference material (CRM) sediment samples. The HS-SPME-GC-PFPD was then applied to the analysis of three harbour sediment samples. The results showed that headspace SPME is an attractive tool for analysis of organotin compounds in solid environmental matrices. (orig.)

  20. The anti-tumour properties and biodistribution (as determined by the radiolabeled equivalent) of Au-compounds intended as potential chemotherapeutics

    Energy Technology Data Exchange (ETDEWEB)

    Nell, M.J. [Department of Pharmacology, University of Pretoria, P.O. Box 2034, Pretoria 0001 (South Africa); Wagener, J.M. [Radiochemistry, NECSA (South African Nuclear Energy Corporation Ltd.), P.O. Box 582, Pretoria 0001 (South Africa)], E-mail: jwagener@necsa.co.za; Zeevaart, J.R. [CARST, North West University, Mafikeng Campus, P. Bag X2046, Mmabatho 2735 (South Africa); Kilian, E. [Department of Pharmacology, Onderstepoort, University of Pretoria, P.O. Box 2034, Pretoria 0001 (South Africa); Mamo, M.A.; Layh, M. [Molecular Sciences Institute, School of Chemistry, University of the Witwatersrand, Private Bag 3, Wits, 2050 Johannesburg (South Africa); Coyanis, M. [Project AuTEK, Mintek, Private Bag X3015, Randburg 2125 (South Africa); Rensburg, C.E.J. van [Department of Pharmacology, University of Pretoria, P.O. Box 2034, Pretoria 0001 (South Africa)

    2009-07-15

    The anti-tumour activity of the Au (I) phosphine complex [Au(dppe{sub 2}]Cl was first discovered in the mid 1980s although promising results were obtained it did not pass clinical studies because of its toxicity to organs such as the liver and heart. The aim of this study was to determine whether the two novel gold compounds (MM5 and MM6), selected for this study, have higher selectivity for cancer cells with less toxicity towards normal cells than [Au(dppe){sub 2}]Cl, and also to determine whether they have improved bio distribution compared to [Au(dppe){sub 2}]Cl. The Au-compounds as potential chemotherapeutic drugs were evaluated by using radioactive tracers in the in vitro and in vivo studies. Results obtained from these experiments showed that the uptake of these experimental compounds was dependent on their octanol/water partition coefficient. However; the inhibition of cell growth did not correlate with the uptake of these compounds by the cells that were tested. In terms of the total uptake it was found that the compounds that were less lipophilic (MM5, MM6) were taken up less efficiently in cells than those that are more lipophilic. Therefore hydrophilic drugs are expected to have a limited biodistribution compared to lipophilic drugs. This might imply a more selective tumour uptake.

  1. An indirect sequential determination of phosphorus and arsenic in high-purity tungsten and its compounds by atomic-absorption spectrophotometry

    International Nuclear Information System (INIS)

    Tekula-Buxbaum, P.

    1981-01-01

    An indirect atomic-absorption spectrophotometric method based on selective extraction of heteropolymolybdic acids has been developed for determination of small quantities of P and As in high-purity tungsten metal and tungsten compounds. The method is suitable for determination of 5-100 ppm of phosphorus and arsenic. The relative standard deviation is 38-5% for P and 31-3% for As, depending on the concentrations. (auth.)

  2. Effectiveness of the compound chlorpyrifos+ cypermethrin+citronellal against Alphitobius diaperinus: laboratory analysis and residue determination in carcasses

    Directory of Open Access Journals (Sweden)

    GS Silva

    2007-09-01

    Full Text Available Effectiveness, biological security and the absence of residues in meat and/or eggs must be considered when recommending options for the control Alphitobius diaperinus in poultry production environments. This research study evaluated the effectiveness of cypermethrin+ chlorpyrifos+citronellal in the control of A. diaperinus, including analysis for the presence of residues of this compound in poultry carcasses (experimental farm. Two studies were carried out under laboratory conditions. One used paper filters a four dilutions of the compound, and the other used a container including with pulverized broiler litter and the compound. The analysis of carcasses for residues was conducted in broilers that raised in a broiler house treated (floor and/or litter with the compound at a dilution of 1:800. Birds were regularly sacrificed, submitted to necropsy, and liver, muscle and fat fragments were collected. Gas chromatography was used to identify the possible presence of any chemical residue in these samples. High effectiveness rates against A.diaperinus were observed in the two laboratory studies, as well as the absence of residues in the carcasses. This compound, used in the studied concentrations, can be recommended as a valuable alternative for the control and treatment of A. diaperinus.

  3. On the use of spectroscopic techniques to determine the crystal structure of compounds of the artificial f elements

    International Nuclear Information System (INIS)

    Peterson, J.R.

    1989-01-01

    For some time the author has been using solid state absorption spectrophotometry to identify the crystal structure of selected transuranium (5f) and promethium (4f) compounds, based on spectral-structural correlations in his data base. More recently he has shown that Raman phonon spectroscopy is also very useful in this regard. These spectral probes of structure have their specific advantages and disadvantages; however, both are applicable to the structural characterization of radioactive compounds and can provide data for interpretation faster and more reliably than the commonly used X-ray powder diffraction method. The experimental methods, examples from the growing data bases, successes and limitations of these spectral probes of crystal structure, and some useful applications to the study of f-element compounds under varying conditions of temperature and pressure are presented

  4. TECHNICAL JUSTIFICATION FOR CHOOSING PROPANE AS A CALIBRATION AGENT FOR TOTAL FLAMMABLE VOLATILE ORGANIC COMPOUND (VOC) DETERMINATIONS

    International Nuclear Information System (INIS)

    DOUGLAS, J.G.

    2006-01-01

    This document presents the technical justification for choosing and using propane as a calibration standard for estimating total flammable volatile organic compounds (VOCs) in an air matrix. A propane-in-nitrogen standard was selected based on a number of criteria: (1) has an analytical response similar to the VOCs of interest, (2) can be made with known accuracy and traceability, (3) is available with good purity, (4) has a matrix similar to the sample matrix, (5) is stable during storage and use, (6) is relatively non-hazardous, and (7) is a recognized standard for similar analytical applications. The Waste Retrieval Project (WRP) desires a fast, reliable, and inexpensive method for screening the flammable VOC content in the vapor-phase headspace of waste containers. Table 1 lists the flammable VOCs of interest to the WRP. The current method used to determine the VOC content of a container is to sample the container's headspace and submit the sample for gas chromatography--mass spectrometry (GC-MS) analysis. The driver for the VOC measurement requirement is safety: potentially flammable atmospheres in the waste containers must be allowed to diffuse prior to processing the container. The proposed flammable VOC screening method is to inject an aliquot of the headspace sample into an argon-doped pulsed-discharge helium ionization detector (Ar-PDHID) contained within a gas chromatograph. No actual chromatography is performed; the sample is transferred directly from a sample loop to the detector through a short, inert transfer line. The peak area resulting from the injected sample is proportional to the flammable VOC content of the sample. However, because the Ar-PDHID has different response factors for different flammable VOCs, a fundamental assumption must be made that the agent used to calibrate the detector is representative of the flammable VOCs of interest that may be in the headspace samples. At worst, we desire that calibration with the selected calibrating

  5. Determination of phases of {alpha} - Fe{sub 2}O{sub 3}: SiO{sub 2} compound by the Rietveld refinement

    Energy Technology Data Exchange (ETDEWEB)

    Palomares S, S.A. [Istituto Materiali Speciali per Elettronica e Magnetismo (MASPEC), Parco Area delle Scienze 37A-43010 Loc. Fontanni, Parma (Italy); Ponce C, S.; Martinez, J.R. [Facultad de Ciencias, Universidad Autonoma de San Luis Potosi, 78000 San Luis Potosi (Mexico); Ruiz, F. [Instituto Potosino de Investigacion Cientifica y Tecnologica, Av. V. Carranza 2025, San Luis Potosi (Mexico)

    2002-07-01

    We use a variation of the Rietveld refinement method to calculate the amorphous content of composites formed by a silica xerogel amorphous matrix and iron particles embedded into. In order to apply the Rietveld refinement to amorphous structures an initial crystalline model is assumed with the same composition as the material to be modelled. In this work we try to refine the structure of compounds using the program MAUD. It is shown how this program can be used to determine the amorphous and crystalline fractions in composites consisting of an amorphous matrix and incorporated iron oxide particles. The analysed compounds underwent different thermal treatments. (Author)

  6. The IP vs. VDE competition as a key factor determining the stability of the MgBX 5 (X = F, Cl) compounds

    Science.gov (United States)

    Sikorska, Celina; Skurski, Piotr

    2010-11-01

    The explanation of the MgBX 5 (X = F, Cl) systems existence and stability is provided on the basis of theoretical considerations supported by ab initio calculations. The equilibrium structures and most probable fragmentation processes of 26 (including isomers) MgBX 5 molecules and six OBX 5 compounds (for comparison) were examined and discussed. The competition between the ionization potential (IP) of the MgX subunit and the electron binding energy (VDE) of the BX 4 fragment was found to be the key factor determining the ability to form a stable compound of MgBX 5 type.

  7. Development of a general model for determination of thermal conductivity of liquid chemical compounds at atmospheric pressure

    DEFF Research Database (Denmark)

    Gharagheizi, Farhad; Ilani‐Kashkouli, Poorandokht; Sattari, Mehdi

    2013-01-01

    In this communication, a general model for representation/presentation of the liquid thermal conductivity of chemical compounds (mostly organic) at 1 atm pressure for temperatures below normal boiling point and at saturation pressure for temperatures above the normal boiling point is developed...... using the Gene Expression Programming algorithm. Approximately 19,000 liquid thermal conductivity data at different temperatures related to 1636 chemical compounds collected from the DIPPR 801 database are used to obtain the model as well as to assess its predictive capability. The parameters...

  8. Molecular determinants of subtype-selective efficacies of cytisine and the novel compound NS3861 at heteromeric nicotinic acetylcholine receptors

    DEFF Research Database (Denmark)

    Harpsøe, Kasper; Hald, Helle; Timmermann, Daniel B

    2013-01-01

    Deciphering which specific agonist-receptor interactions affect efficacy levels is of high importance, because this will ultimately aid in designing selective drugs. The novel compound NS3861 and cytisine are agonists of nicotinic acetylcholine receptors (nAChRs) and both bind with high affinity...

  9. Human breath measurements in a clean-air chamber to determine half-lives for volatile organic compounds

    Science.gov (United States)

    Gordon, Sydney M.; Wallace, Lance A.; Pelllzzari, Edo D.; O'Neill, Hugh J.

    The expired breath of four non-occupationally exposed subjects was monitored following exposure at near-normal environmental concentrations using a specially developed pulmonary clearance technique. The four were exposed to polluted air on a heavily trafficked freeway or at a local dry-cleaning establishment, then spent the next 10 h in a clean-air environmental chamber. Breath and chamber-air samples were collected at regular intervals throughout the 10-h period and analyzed for the presence of selected target compounds. The breath levels of two of the compounds were elevated and decreased slowly with time once the subjects began to breathe clean air. Nonlinear least-squares fitting of the decay-uptake curves permitted the calculation of biological half-lives. Several of the target compounds occurred, however, at very low levels, and the resultant experimental scatter limited the value of these measurements. Higher initial exposures to most of the target compounds would have improved the reliability of the estimates.

  10. Work Tasks as Determinants of Grain Dust and Microbial Exposure in the Norwegian Grain and Compound Feed Industry

    NARCIS (Netherlands)

    Straumfors, Anne; Heldal, Kari Kulvik; Wouters, Inge M; Eduard, Wijnand

    OBJECTIVES: The grain and compound feed industry entails inevitable risks of exposure to grain dust and its microbial content. The objective of this study was therefore to investigate task-dependent exposure differences in order to create knowledge basis for awareness and exposure reducing measures

  11. Composition of sulla (Hedysarum coronarium L.) honey solvent extractives determined by GC/MS: norisoprenoids and other volatile organic compounds.

    Science.gov (United States)

    Jerković, Igor; Tuberoso, Carlo I G; Tuberso, Carlo I G; Gugić, Mirko; Bubalo, Dragan

    2010-09-09

    Samples of unifloral sulla (Hedysarum coronarum L.) honey from Sardinia (Italy) were analysed. To investigate the chemical composition of the honey volatiles two solvent systems were used for ultrasonic solvent extraction (USE): 1) a 1:2 (v/v) pentane and diethyl ether mixture and 2) dichloromethane. All the extracts were analysed by GC and GC/MS. These procedures have permitted the identification of 56 compounds that include norisoprenoids, benzene derivatives, aliphatic compounds and Maillard reaction products. Norisoprenoids were the major compounds in both extracts, dominated by vomifoliol (5.3-11.2%; 9.6-14.0%) followed by minor percentages of other norisoprenoids such as α-isophorone, 4-ketoisophorone, 3-oxo-α-ionol or 3-oxo-α-ionone. Other abundant single compounds in the extracts were 3-hydroxy-4-phenylbutan-2-one (0.8-5.4%; 0.6-5.7%) and methyl syringate (3.0-5.7%; 2.2-4.1%). The composition of the volatiles and semi-volatiles in the obtained extracts suggests that sulla honey is quite distinctive relative to the other honeys that have been chemically studied by GC/MS, but no specific markers of the honey botanical origin were found.

  12. Composition of Sulla (Hedysarum coronarium L. Honey Solvent Extractives Determined by GC/MS: Norisoprenoids and Other Volatile Organic Compounds

    Directory of Open Access Journals (Sweden)

    Dragan Bubalo

    2010-09-01

    Full Text Available Samples of unifloral sulla (Hedysarum coronarum L. honey from Sardinia (Italy were analysed. To investigate the chemical composition of the honey volatiles two solvent systems were used for ultrasonic solvent extraction (USE: 1 a 1:2 (v/v pentane and diethyl ether mixture and 2 dichloromethane. All the extracts were analysed by GC and GC/MS. These procedures have permitted the identification of 56 compounds that include norisoprenoids, benzene derivatives, aliphatic compounds and Maillard reaction products. Norisoprenoids were the major compounds in both extracts, dominated by vomifoliol (5.3-11.2%; 9.6-14.0% followed by minor percentages of other norisoprenoids such as α-isophorone, 4-ketoisophorone, 3-oxo-α-ionol or 3-oxo-α-ionone. Other abundant single compounds in the extracts were 3-hydroxy-4-phenylbutan-2-one (0.8-5.4%; 0.6-5.7% and methyl syringate (3.0-5.7%; 2.2-4.1%. The composition of the volatiles and semi-volatiles in the obtained extracts suggests that sulla honey is quite distinctive relative to the other honeys that have been chemically studied by GC/MS, but no specific markers of the honey botanical origin were found.

  13. Determination of indole alkaloids and highly volatile compounds in Rauvolfia verticillata by HPLC-UV and GC-MS.

    Science.gov (United States)

    Hong, Bo; Li, Wenjing; Song, Aihua; Zhao, Chunjie

    2013-01-01

    Rauvolfia verticillata (Lour.) Baill. (also called Luofumu in Chinese) is commonly used in traditional Chinese medicine for lowering blood pressure. In this study, a high-performance liquid chromatography assay using ultraviolet detection is described for the simultaneous measurement of the five bioactive indole alkaloids (sarpagine, yohimbine, ajmaline, ajmalicine and reserpine) in Rauvolfia. The detection of all five compounds was conducted at 280 nm. In quantitative analysis, the five compounds showed good regressions (R(2) > 0.9988) within the test ranges, and the recovery of the method was in the range of 90.4-101.4%. In addition, a simple gas chromatography mass method using a DB-1 silica capillary column (30 m × 0.25 mm i.d., 0.25 µm) is described for the identification of the highly volatile compounds in Rauvolfia. In qualitative analysis, more than 39 compounds were assayed and identified using the mass function and the National Institute of Standards and Technology database search system. The results demonstrated that the combination of quantitative and qualitative analyses offered an efficient way to evaluate the quality and consistency of Rauvolfia verticillata.

  14. Solid-phase extraction element based on epoxy polymer monolith for determination of polar organic compounds in aqueous media.

    Science.gov (United States)

    Takahashi, Tadashi; Odagiri, Kayo; Watanabe, Atsushi; Watanabe, Chuichi; Kubo, Takuya; Hosoya, Ken

    2011-10-01

    A solid-phase extraction element based on epoxy polymer monolith was fabricated for sorptive enrichment of polar compounds from liquid and gaseous samples. After ultrasonication of the element in an aqueous solution for a given period of time, the thermal desorption (TD) using a pyrolyzer with gas chromatography/mass spectrometry (GC/MS), in which TD temperature was programmed from 50 to 250 °C for the analytes absorbed in the element, was used to evaluate the element for basic extraction performance using the aqueous standard mixtures consisting of compounds having varied polarities such as hexanol, isoamyl acetate, linalool, furfural and decanoic acid, in concentrations ranging from 10 μg/L to 1 mg/L. Excellent linear relationships were observed for all compounds in the standard mixture, except decanoic acid. In the extraction of beverages such as red wine, the extraction element showed stronger adsorption characteristics for polar compounds such as alcohols and acids than a non-polar polydimethylsiloxane-based element. This feature is derived from the main polymer structure along with hydroxyl and amino groups present in the epoxy-based monolith polymer matrix. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Fast gradient HPLC method to determine compounds binding to human serum albumin. Relationships with octanol/water and immobilized artificial membrane lipophilicity.

    Science.gov (United States)

    Valko, Klara; Nunhuck, Shenaz; Bevan, Chris; Abraham, Michael H; Reynolds, Derek P

    2003-11-01

    A fast gradient HPLC method (cycle time 15 min) has been developed to determine Human Serum Albumin (HSA) binding of discovery compounds using chemically bonded protein stationary phases. The HSA binding values were derived from the gradient retention times that were converted to the logarithm of the equilibrium constants (logK HSA) using data from a calibration set of molecules. The method has been validated using literature plasma protein binding data of 68 known drug molecules. The method is fully automated, and has been used for lead optimization in more than 20 company projects. The HSA binding data obtained for more than 4000 compounds were suitable to set up global and project specific quantitative structure binding relationships that helped compound design in early drug discovery. The obtained HSA binding of known drug molecules were compared to the Immobilized Artificial Membrane binding data (CHI IAM) obtained by our previously described HPLC-based method. The solvation equation approach has been used to characterize the normal binding ability of HSA, and this relationship shows that compound lipophilicity is a significant factor. It was found that the selectivity of the "baseline" lipophilicity governing HSA binding, membrane interaction, and octanol/water partition are very similar. However, the effect of the presence of positive or negative charges have very different effects. It was found that negatively charged compounds bind more strongly to HSA than it would be expected from the lipophilicity of the ionized species at pH 7.4. Several compounds showed stronger HSA binding than can be expected from their lipophilicity alone, and comparison between predicted and experimental binding affinity allows the identification of compounds that have good complementarities with any of the known binding sites. Copyright 2003 Wiley-Liss, Inc. and the American Pharmacists Association J Pharm Sci 92:2236-2248, 2003

  16. Determination of a wide range of volatile organic compounds in ambient air using multisorbent adsorption/thermal desorption and gas chromatography/mass spectrometry

    Science.gov (United States)

    Pankow, J.F.; Luo, W.; Isabelle, L.M.; Bender, D.A.; Baker, R.J.

    1998-01-01

    Adsorption/thermal desorption with multisorbent air-sampling cartridges was developed for the determination of 87 method analytes including halogenated alkanes, halogenated alkenes, ethers, alcohols, nitriles, esters, ketones, aromatics, a disulfide, and a furan. The volatilities of the compounds ranged from that of dichlorofluoromethane (CFC12) to that of 1,2,3- trichlorobenzene. The eight most volatile compounds were determined using a 1.5-L air sample and a sample cartridge containing 50 mg of Carbotrap B and 280 mg of Carboxen 1000; the remaining 79 compounds were determined using a 5-L air sample and a cartridge containing 180 mg of Carbotrap B and 70 mg of Carboxen 1000. Analysis and detection were by gas chromatography/mass spectrometry. The minimum detectable level (MDL) concentration values ranged from 0.01 parts per billion by volume (ppbv) for chlorobenzene to 0.4 ppbv for bromomethane; most of the MDL values were in the range 0.02-0.06 ppbv. No breakthrough was detected with the prescribed sample volumes. Analyte stability on the cartridges was very good. Excellent recoveries were obtained with independent check standards. Travel spike recoveries ranged from 90 to 110% for 72 of the 87 compounds. The recoveries were less than 70% for bromomethane and chloroethene and for a few compounds such as methyl acetate that are subject to losses by hydrolysis; the lowest travel spike recovery was obtained for bromomethane (62%). Blank values for all compounds were either below detection or very low. Ambient atmospheric sampling was conducted in New Jersey from April to December, 1997. Three sites characterized by low, moderate, and high densities of urbanization/traffic were sampled. The median detected concentrations of the compounds were either similar at all three sites (as with the chlorofluorocarbon compounds) or increased with the density of urbanization/traffic (as with dichloromethane, MTBE, benzene, and toluene). For toluene, the median detected

  17. Antioxidant and Anti-Inflammatory Activity Determination of One Hundred Kinds of Pure Chemical Compounds Using Offline and Online Screening HPLC Assay

    Directory of Open Access Journals (Sweden)

    Kwang Jin Lee

    2015-01-01

    Full Text Available This study investigated the antioxidant activity of one hundred kinds of pure chemical compounds found within a number of natural substances and oriental medicinal herbs (OMH. Three different methods were used to evaluate the antioxidant activity of DPPH radical-scavenging activity, ABTS radical-scavenging activity, and online screening HPLC-ABTS assays. The results indicated that 17 compounds exhibited better inhibitory activity against ABTS radical than DPPH radical. The IC50 rate of a more practical substance is determined, and the ABTS assay IC50 values of gallic acid hydrate, (+-catechin hydrate, caffeic acid, rutin hydrate, hyperoside, quercetin, and kaempferol compounds were 1.03 ± 0.25, 3.12 ± 0.51, 1.59 ± 0.06, 4.68 ± 1.24, 3.54 ± 0.39, 1.89 ± 0.33, and 3.70 ± 0.15 μg/mL, respectively. The ABTS assay is more sensitive to identifying the antioxidant activity since it has faster reaction kinetics and a heightened response to antioxidants. In addition, there was a very small margin of error between the results of the offline-ABTS assay and those of the online screening HPLC-ABTS assay. We also evaluated the effects of 17 compounds on the NO secretion in LPS-stimulated RAW 264.7 cells and also investigated the cytotoxicity of 17 compounds using a cell counting kit (CCK in order to determine the optimal concentration that would provide an effective anti-inflammatory action with minimum toxicity. These results will be compiled into a database, and this method can be a powerful preselection tool for compounds intended to be studied for their potential bioactivity and antioxidant activity related to their radical-scavenging capacity.

  18. Thin-film microextraction coupled to LC-ESI-MS/MS for determination of quaternary ammonium compounds in water samples.

    Science.gov (United States)

    Boyacı, Ezel; Sparham, Chris; Pawliszyn, Janusz

    2014-01-01

    The dual nature of the quaternary ammonium compounds, having permanently charged hydrophilic quaternary ammonium heads and long-chain hydrophobic tails, makes the sample preparation step and analysis of these compounds challenging. A high-throughput method based on thin-film solid-phase microextraction (SPME) and liquid chromatography mass spectrometry was developed for simultaneous quantitative analysis of nine benzylic and aliphatic quaternary ammonium compounds. Chromatographic separation and detection of analytes were obtained in reverse-phase mode in 8 min using a triple quadrupole mass spectrometer. Hydrophilic lipophilic balance particle-coated blades were found to be the most suitable among the different coatings tested in terms of recoveries and carryover on the blades. For desorption solvents, 70/30, v/v (A/B) with 0.1 % formic acid (where A is 10 mM ammonium acetate in acetonitrile/water (95/5 , v/v) and B is 0.1 %  (v/v) formic acid in isopropyl alcohol) was shown to be the most efficient solvent for the desorption of the analytes from the SPME sorbent. The SPME method was optimised in terms of extraction, pH, and preconditioning, as well as extraction and desorption times. Optimum conditions were 45 min of extraction time and 15 min of desorption time, all with agitation. The extraction was found to be optimum in a range of pH 6.0 to 8.0, which is consistent with the natural pH of water samples. Wide linear dynamic ranges with the developed method were obtained for each compound, enabling the application of the method for a wide range of concentrations. The developed method was validated according to the Food and Drug Administration criteria. The proposed method is the first SPME-based approach describing the applicability of the high-throughput thin-film SPME in a 96-well system for analysis of such challenging compounds.

  19. Rapid Determination of Six Low Molecular Carbonyl Compounds in Tobacco Smoke by the APCI-MS/MS Coupled to Data Mining

    Directory of Open Access Journals (Sweden)

    Wuduo Zhao

    2017-01-01

    Full Text Available A simple method was established for the rapid determination of low molecular carbonyl compounds by the combination of atmospheric pressure chemical ionization tandem mass spectrometry (APCI-MS/MS and data mining. The ionization was carried out in positive mode, and six low molecular carbonyl compounds of acrolein, acetone, propionaldehyde, crotonaldehyde, butanone, and butyraldehyde were analyzed by both full scan mode and daughter scan mode. To overcome the quantitative difficulties from isomer of acetone/propionaldehyde and butanone/butyraldehyde, the quantitation procedure was performed with the characteristic ion of [CH3O]+ under CID energy of 5 and 15 eV. Subsequently, the established method was successfully applied to analysis of six low molecular carbonyl compounds in tobacco smoke with analytical period less than four minutes. The contents of acrolein, acetone, propionaldehyde, crotonaldehyde, butanone, and butyraldehyde for a cigarette were about 63±5.8, 325±82, 55±9.7, 11±1.4, 67±5.9, and 12±1.8 μg/cig, respectively. The experimental results indicated that the established method had the potential application in rapid determination of low molecular carbonyl compounds.

  20. Determination of Acetylcholinesrase and Butrylcholinestrase Activities in Whole Blood and Plasma from Different Communities of Khosestan Province (Iran-Iraq War Area) Exposed to Organophosphate Compounds

    International Nuclear Information System (INIS)

    Heybatullah, K.; Jahangiri, A.; Mohebbi, G. H.

    2007-01-01

    It is well known that Organophosphate Compounds are widely used as pesticides. Therefore while handling, applying or using these compounds care and safe use should be considered. The main mechanism of toxicity action of Organophosphate Compounds is the inhibition of Actylcholinestrase and Butrylcholinesrase enzymes. It is well known that the activity measurement of Acetylcholinestrase in whole blood and Butrylcholinestrase in plasma samples are potential biomarker of exposure to Organophosphates compounds.In this study AchE and BchE activities were determined in whole blood and plasma samples of farmers from two different area of Khosestan province of Iran Gotvand and Dashte Azadegan (Iran-Iraq war zone).Determination of enzymes activities were based on the Ellman colorimetric method which was modified byWorek et al. The results obtained in this study showed that Gotvand area showed lower than normal value and Dashte Azadegan (war area) were significantly lower than the mean of activities in reference group (P less than 0.05). Also results of this study showed Acetylcholinestrase and Butrylcholinestrase inhibition can provide a good biomarker of exposure to OP pesticides in field studies in human population with consideration of other different parameters and factors which will be discussed. (author)

  1. Volatile organic compound (VOC) determination in working atmospheres; Determinacion de compuestos organicos volatiles (VOC) en ambiente laboral

    Energy Technology Data Exchange (ETDEWEB)

    Blass A, Georgina; Panama T, Luz A; Corrales C, Deyanira [Instituto de Investigaciones Electricas, Cuernavaca, Morelos (Mexico)

    2003-07-01

    The present work describes, in a synthesized way, the implementation and application of procedures based on the normativity related to the subject of the volatile organic compounds (Volatile Organic Compounds VOC), that allow to sample, quantify and evaluate the present contamination in the working atmosphere of a refinery due to the fugitive emissions of VOC and other substances. In accordance with the corresponding normativity, more than 189 organic compounds denominated dangerous air polluting agents (Hazardous Air Pollutants, HAP) can be found in a working atmosphere, but they are the 11 main HAP that can be found in a refinery. In the present article the work made for the sampling and quantification of 5 of the 11 dangerous polluting agents of the air: benzene, toluene, xylene, iso-octane and naphthalene. [Spanish] El presente trabajo describe, de manera sintetizada, la implementacion y aplicacion de procedimientos basados en la normatividad relacionada al tema de los compuestos organicos volatiles (Volatil Organic Compounds, VOC), que permiten muestrear, cuantificar y evaluar la contaminacion presente en el ambiente laboral de una refineria debido a las emisiones fugitivas de VOC y otras sustancias. De acuerdo con la normatividad correspondiente, mas de 189 compuestos organicos denominados contaminantes peligrosos del aire (Hazardous Air Pollutants, HAP), pueden ser encontrados en un ambiente laboral, pero son 11 los principales HAP que pueden ser hallados en una refineria. En el presente articulo se informa el trabajo realizado para el muestreo y cuantificacion de 5 de los 11 contaminantes peligrosos del aire: benceno, tolueno, xileno, iso-octano y naftaleno.

  2. HPLC-Analysis of Polyphenolic Compounds in Gardenia jasminoides and Determination of Antioxidant Activity by Using Free Radical Scavenging Assays

    OpenAIRE

    Riaz Uddin; Moni Rani Saha; Nusrat Subhan; Hemayet Hossain; Ismet Ara Jahan; Raushanara Akter; Ashraful Alam

    2014-01-01

    Purpose: Gardenia jasminoides is a traditional medicinal plant rich in anti-inflammatory flavonoids and phenolic compounds and used for the treatment of inflammatory diseases and pain. In this present study, antioxidant potential of Gardenia jasminoides leaves extract was evaluated by using various antioxidant assays. Methods: Various antioxidant assays such as 1, 1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging assay, reducing power and total antioxidant capacity expressed as equival...

  3. Enhancing and inhibiting effects of aromatic compounds on luminol-dimethylsulfoxide-OH(-) chemiluminescence and determination of intermediates in oxidative hair dyes by HPLC with chemiluminescence detection.

    Science.gov (United States)

    Zhou, Jian; Xu, Hong; Wan, Guo-Hui; Duan, Chun-Feng; Cui, Hua

    2004-10-08

    The effect of 36 aromatic compounds on the luminol-dimethylsulfoxide-OH(-) chemiluminescence (CL) was systematically studied. It was found that dihydroxybenzenes, and ortho- and para-substituted aminophenols and phenylenediamines inhibited the CL and phenols with three or more than three hydroxyls except phloroglucin tended to enhance the CL. The CL inhibition and enhancement was proposed to be dependent on whether superoxide anion radical (O(2)(-)) was competitively consumed by compounds in the CL system. Trihydroxybenzenes were capable of generating superoxide anion radical, leading to the CL enhancement, whereas dihydroxybenzenes were superoxide anion radical scavenger, causing the CL inhibition. Based on the inhibited CL, a novel method for the simultaneous determination of p-phenylenediamine, o-phenylenediamine, p-aminophenol, o-aminophenol, resorcinol and hydroquinone by high-performance liquid chromatography coupled with chemiluminescence detection was developed. The method has been successfully applied to determine intermediates in oxidative hair dyes and wastewater of shampooing after hair dyed.

  4. Preparation of biosensors by immobilization of polyphenol oxidase in conducting copolymers and their use in determination of phenolic compounds in red wine.

    Science.gov (United States)

    Böyükbayram, A Elif; Kiralp, Senem; Toppare, Levent; Yağci, Yusuf

    2006-10-01

    Electrochemically produced graft copolymers of thiophene capped polytetrahydofuran (TPTHF1 and TPTHF2) and pyrrole were achieved by constant potential electrolysis using sodium dodecylsulfate (SDS) as the supporting electrolyte. Characterizations were based on Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). Electrical conductivities were measured by the four-probe technique. Novel biosensors for phenolic compounds were constructed by immobilizing polyphenol oxidase (PPO) into conducting copolymers prepared by electropolymerization of pyrrole with thiophene capped polytetrahydrofuran. Kinetic parameters, maximum reaction rate (V(max)) and Michaelis-Menten constant (K(m)) and optimum conditions regarding temperature and pH were determined for the immobilized enzyme. Operational stability and shelf-life of the enzyme electrodes were investigated. Enzyme electrodes of polyphenol oxidase were used to determine the amount of phenolic compounds in two brands of Turkish red wines and found very useful owing to their high kinetic parameters and wide pH working range.

  5. Determination of musks and other fragrance compounds at ng/L levels using CLSA (closed loop stripping analysis) and GC/MS detection.

    Science.gov (United States)

    Mitjans, D; Ventura, F

    2004-01-01

    Closed loop stripping analysis (CLSA), a suitable tool for the determination of volatile and semivolatile compounds at low trace levels (ng/l), has been used to determine and quantify seven selected musks and two fragrances (Acetyl cedrene and Amberonne). The obtained extracts are analyzed by high resolution gas chromatography coupled to mass spectrometry (GC/MS) operating in the SIM mode. Quality parameters such as limit of detection; matrix effects; precision expressed as repeatability and reproducibility relative standard deviations of the method and an estimation of the uncertainty have been evaluated. The method has been applied to the analysis of wastewater effluents, surface water and tap water from different places in Europe. All samples contained differents musks at ng/l levels with the polycyclic musks Galaxolide and Tonalide and both fragrances, Amberonne and Acetyl cedrene, being the most abundant. These results suggest the importance of studying and controlling the presence of these ubiquitous environmental compounds in water systems.

  6. Determination of pharmaceutical compounds in surface- and ground-water samples by solid-phase extraction and high-performance liquid chromatography-electrospray ionization mass spectrometry

    Science.gov (United States)

    Cahill, J.D.; Furlong, E.T.; Burkhardt, M.R.; Kolpin, D.; Anderson, L.G.

    2004-01-01

    Commonly used prescription and over-the-counter pharmaceuticals are possibly present in surface- and ground-water samples at ambient concentrations less than 1 μg/L. In this report, the performance characteristics of a combined solid-phase extraction isolation and high-performance liquid chromatography–electrospray ionization mass spectrometry (HPLC–ESI-MS) analytical procedure for routine determination of the presence and concentration of human-health pharmaceuticals are described. This method was developed and used in a recent national reconnaissance of pharmaceuticals in USA surface waters. The selection of pharmaceuticals evaluated for this method was based on usage estimates, resulting in a method that contains compounds from diverse chemical classes, which presents challenges and compromises when applied as a single routine analysis. The method performed well for the majority of the 22 pharmaceuticals evaluated, with recoveries greater than 60% for 12 pharmaceuticals. The recoveries of angiotensin-converting enzyme inhibitors, a histamine (H2) receptor antagonist, and antihypoglycemic compound classes were less than 50%, but were retained in the method to provide information describing the potential presence of these compounds in environmental samples and to indicate evidence of possible matrix enhancing effects. Long-term recoveries, evaluated from reagent-water fortifications processed over 2 years, were similar to initial method performance. Method detection limits averaged 0.022 μg/L, sufficient for expected ambient concentrations. Compound-dependent matrix effects on HPLC/ESI-MS analysis, including enhancement and suppression of ionization, were observed as a 20–30% increase in measured concentrations for three compounds and greater than 50% increase for two compounds. Changing internal standard and more frequent ESI source maintenance minimized matrix effects. Application of the method in the national survey demonstrates that several

  7. Determination of Chemical Compounds Generated from Second-generation E-cigarettes Using a Sorbent Cartridge Followed by a Two-step Elution Method.

    Science.gov (United States)

    Uchiyama, Shigehisa; Senoo, Yui; Hayashida, Hideki; Inaba, Yohei; Nakagome, Hideki; Kunugita, Naoki

    2016-01-01

    We developed an analytical method for analyzing electronic cigarette (E-cigarette) smoke, and measured the carbonyl compounds and volatile organic compounds generated by 10 brands of second-generation E-cigarettes. A glass filter (Cambridge filter pad) for particulate matter and a solid sorbent tube packed with Carboxen-572 for gaseous compounds were used to collect E-cigarette smoke. These were then analyzed using a two-step elution method with carbon disulfide and methanol, followed by high-performance liquid chromatography (HPLC) and gas chromatography mass spectrometry (GC/MS). Formaldehyde (FA), acetaldehyde (AA), acetone (AC), acrolein (ACR), propanal (PA), acetol (AT), glyoxal (GO), and methyl glyoxal (MGO) were detected by HPLC in some E-cigarettes. Propylene glycol (PG), glycerol (GLY), and some esters were detected by GC/MS. GO and MGO exist mainly as particulate matter. AA, AC, ACR, PA, and AT exist mainly as gaseous compounds. FA exists as both particulate matter and gaseous compounds. These carbonyl compounds have carbon numbers C1 - C3. The main components of E-liquid are PG (C3) and GLY (C3). Therefore, the oxidation of liquids, such as PG and GLY in E-cigarettes upon incidental contact with the heating element in E-cigarette, is suggested as being a possible cause for carbonyl generation. When the puff number exceeds a critical point, carbonyl generation rapidly increases and then remains constant. The results of this study are now being used to determine the following E-cigarette smoking protocol: puff volume, 55 mL; puff duration, 2 s; and puff number, 30. E-cigarette analysis revealed very large variation in carbonyl concentration among not only different brands, but also different samples of the same product. Typical distributions of carbonyl concentration were not observed in any of the E-cigarettes tested, and the mean values greatly differed from median values.

  8. Innovative method of direct determination of the content of paraffins, naphthenes, aromatics and sulfur compounds by capillary high-resolution gas chromatography

    Directory of Open Access Journals (Sweden)

    R. Baizhumanova

    2012-03-01

    Full Text Available Based on determination of individual Hydrocarbon (paraffins, naphthenes, aromatics and Sulphur components of fuels and their mixture on the thin bonded of absorber (the stationary phase is a 100-metre silica capillary column, containing 0.5μm film thickness of bonded dimethylpolysiloxane phase by means of the selective solvents (mobile phase combined with technique of ionization of separated compounds by Flame Ionization Detector (FID and Sulphur Chemiluminescence Detector (SCD.

  9. Dioxins and dioxin-like compounds in composts and digestates from European countries as determined by the in vitro bioassay and chemical analysis.

    Science.gov (United States)

    Beníšek, Martin; Kukučka, Petr; Mariani, Giulio; Suurkuusk, Gert; Gawlik, Bernd M; Locoro, Giovanni; Giesy, John P; Bláha, Luděk

    2015-03-01

    Aerobic composting and anaerobic digestion plays an important role in reduction of organic waste by transforming the waste into humus, which is an excellent soil conditioner. However, applications of chemical-contaminated composts on soils may have unwanted consequences such as accumulation of persistent compounds and their transfer into food chains. The present study investigated burden of composts and digestates collected in 16 European countries (88 samples) by the compounds causing dioxin-like effects as determined by use of an in vitro transactivation assay to quantify total concentrations of aryl hydrocarbon receptor-(AhR) mediated potency. Measured concentrations of 2,3,7,8-Tetrachlorodibeno-p-dioxin (2,3,7,8-TCDD) equivalents (TEQbio) were compared to concentrations of polycyclic aromatic hydrocarbons (PAHs) and selected chlorinated compounds, including polychlorinated dibenzo-p-dioxins/furans (PCDD/Fs), co-planar polychlorinated biphenyls (PCBs), indicator PCB congeners and organochlorine pesticides (OCPs). Median concentrations of TEQbio (dioxin-like compounds) determined by the in vitro assay in crude extracts of various types of composts ranged from 0.05 to 1.2 with a maximum 8.22μg (TEQbio)kg(-1) dry mass. Potencies were mostly associated with less persistent compounds such as PAHs because treatment with sulfuric acid removed bioactivity from most samples. The pan-European investigation of contamination by organic contaminants showed generally good quality of the composts, the majority of which were in compliance with conservative limits applied in some countries. Results demonstrate performance and added value of rapid, inexpensive, effect-based monitoring, and points out the need to derive corresponding effect-based trigger values for the risk assessment of complex contaminated matrices such as composts. Copyright © 2014 Elsevier Ltd. All rights reserved.

  10. Determination of selected quaternary ammonium compounds by liquid chromatography with mass spectrometry. Part II. Application to sediment and sludge samples in Austria

    International Nuclear Information System (INIS)

    Martinez-Carballo, Elena; Gonzalez-Barreiro, Carmen; Sitka, Andrea; Kreuzinger, Norbert; Scharf, Sigrid; Gans, Oliver

    2007-01-01

    Soxhlet extraction and high-performance liquid chromatography (HPLC) coupled to tandem mass spectrometry detection (MS/MS) was used for the determination of selected quaternary ammonium compounds (QACs) in solid samples. The method was applied for the determination of alkyl benzyl, dialkyl and trialkyl quaternary ammonium compounds in sediment and sludge samples in Austria. The overall method quantification limits range from 0.6 to 3 μg/kg for sediments and from 2 to 5 μg/kg for sewage sludges. Mean recoveries between 67% and 95% are achieved. In general sediments were especially contaminated by C12 chain benzalkonium chloride (BAC-C12) as well as by the long C-chain dialkyldimethylammonium chloride (DDAC-C18) with a maximum concentration of 3.6 mg/kg and 2.1 mg/kg, respectively. Maxima of 27 mg/kg for DDAC-C10, 25 mg/kg for BAC-C12 and 23 mg/kg for BAC-C14 were determined for sludge samples. The sums of the 12 selected target compounds range from 22 mg/kg to 103 mg/kg in the sludge samples. - The presence of quaternary ammonium surfactants in sediment and sludge samples is reported for the first time in Austria

  11. Determination of the mechanism of demethylenation of (methylenedioxy)phenyl compounds by cytochrome P450 using deuterium isotope effects

    International Nuclear Information System (INIS)

    Fukuto, J.M.; Kumagai, Y.; Cho, A.K.

    1991-01-01

    The mechanism of demethylenation of (methylenedioxy)benzene (MDB), (methylenedioxy)amphetamine (MDA), and (methylenedioxy)methamphetamine (MDMA) by purified rabbit liver cytochrome P450IIB4 has been investigated by using deuterium isotope effects. A comparison of the magnitude and direction of the observed kinetic isotope effects indicates that the three compounds are demethylenated by different mechanisms. The different mechanisms of demethylenation have been proposed on the basis of comparisons of the observed biochemical isotope effects with the isotope effects from purely chemical systems

  12. Determination of concentration of radon, volatile organic compounds (VOC) and water chemistry in springs near to Popocatepetl volcano

    International Nuclear Information System (INIS)

    Pena, P.; Segovia, N.; Lopez M, B.E.; Cisniega, G.; Valdes, C.; Armienta, M.A.; Mena, M.

    2004-01-01

    Popocatepetl volcano is a high-risk active volcano in Central Mexico where the highest population density in the country is settled. Radon in the soil and groundwater together with water chemistry from samples of nearby springs is analysed as a function of the 2002-2003 volcanic activity. Soil radon indicated fluctuations related both the meteorological parameters and sporadic explosive events. Groundwater radon showed essentially differences in concentration due to the specific characteristics of the studied springs. Water chemistry showed stability along the monitoring period indicating also differences between springs. No anthropogenic pollution from volatile organic compounds was observed. (Author)

  13. An efficient and economical MTT assay for determining the antioxidant activity of plant natural product extracts and pure compounds.

    Science.gov (United States)

    Liu, Yunbao; Nair, Muraleedharan G

    2010-07-23

    Antioxidants scavenge free radicals, singlet oxygen, and electrons in cellular redox reactions. The yellow MTT [3-(4,5-dimethylthiazole-2-yl)-2,5-diphenyltetrazolium bromide] is reduced to a purple formazan by mitochondrial enzymes. NADPH is the basis of established in vitro cell viability assays. An antioxidant assay has been developed utilizing the redox reaction between MTT and selected natural product extracts and purified compounds. This simple, fast, and inexpensive MTT antioxidant assay is comparable with the lipid peroxidation inhibitory assay and can be mechanized to achieve high throughput.

  14. Determination of octanol-water partition coefficients of polar polycyclic aromatic compounds (N-PAC) by high performance liquid chromatography

    DEFF Research Database (Denmark)

    Helweg, C.; Nielsen, T.; Hansen, P.E.

    1997-01-01

    Prediction of 1-octanol water partition coefficients for a range of polar N-PAC from HPLC capacity coefficients has been investigated. Two commercially available columns, an ODS column and a Diol column were tested with water-methanol eluents. The best prediction of log K-ow for N-PAC was achieve...... with size and log K-ow for N-PAC was 1.1-1.3 lower than log K-ow for the equivalent PAH. Shielding of the nitrogen atom in the N-PAC compounds caused an increase in log K-ow. (C) 1997 Elsevier Science Ltd....

  15. MCX based solid phase extraction combined with liquid chromatography tandem mass spectrometry for the simultaneous determination of 31 endocrine-disrupting compounds in surface water of Shanghai.

    Science.gov (United States)

    Zhang, Hong-Chang; Yu, Xue-jun; Yang, Wen-chao; Peng, Jin-feng; Xu, Ting; Yin, Da-Qiang; Hu, Xia-lin

    2011-10-15

    A novel analytical method employing MCX (mixed-mode cationic exchange) based solid phase extraction (SPE) coupled with liquid chromatography tandem mass spectrometry (LC-MS/MS) was developed to detect 31 endocrine-disrupting compounds (EDCs) in surface water samples simultaneously. The target EDCs belong to five classes, including seven estrogens, eight androgens, six progesterones, five adrenocortical hormones and five industrial compounds. In order to simultaneously concentrate the target EDCs and eliminate matrix interferences in the water samples, MCX SPE cartridges were employed for SPE, and then followed by a simple and highly efficient three-step sequential elution procedure. Two electrospray ionization (ESI) detection modes, positive (ESI+) and (ESI-), were optimized for HPLC-MS/MS analysis to obtain the highest sensitivity for all the EDCs. The limits of detection (LODs) were 0.02-1.9 ng L(-1), which are lower than or comparable to these reported in references. Wide linear ranges (LOD-100 ng L(-1) for ESI+ mode, and LOD-200 ng L(-1) for ESI- mode) were obtained with determination coefficients (R(2)) higher than 0.99 for all the compounds. With five internal standards, good recoveries (84.4-103.0%) of all the target compounds were obtained in selected surface water samples. The developed method was successfully applied to investigate the EDCs occurrence in the surface water of Shanghai by analyzing surface water samples from 11 sites. The results showed that nearly all the target compounds (30 in 31) were present in the surface water samples of Shanghai, of which three industrial compounds (4-t-OP, BPA, and BPF) showed the highest concentrations (median concentrations were 11.88-23.50 ng L(-1)), suggesting that industrial compounds were the dominating EDCs in the surface water of Shanghai, and much more attention should be paid on these compounds. Our present research demonstrated that SPE with MCX cartridges combined with HPLC-MS/MS was convenient

  16. Selective determination of semi-volatile thiophene compounds in water by molecularly imprinted polymer thin films with direct headspace gas chromatography sulfur chemiluminescence detection.

    Science.gov (United States)

    Hijazi, Hassan Y; Bottaro, Christina S

    2018-02-26

    Water-compatible molecularly imprinted polymer (MIP) thin films are coupled with headspace gas chromatography sulfur chemiluminescence detection (HS-GC-SCD) to create a new approach for the determination of trace concentrations of thiophene compounds in water samples. Thiophene compounds are persistent, typically petrogenic, organic pollutants of concern due to their potential for biomagnification and bioaccumulation, mutagenicity, and carcinogenicity in terrestrial and aquatic fauna. Identification and quantitation in water, particularly following oil spills, is a priority. Following adsorption of the thiophenes to the MIPs, the MIP-bound analytes are analyzed directly by HS-GC-SCD, with minimal sample manipulation and virtually no organic solvent. Calibration curves of spiked seawater were linear from 5 μg L -1 to 100 μg L -1 and limits of detection (LOD) were in the range of 0.24-0.82 μg L -1 . Low matrix effects were observed in the analysis of thiophene compounds in seawater making the method suitable for use in fresh and saline waters without modification. Acceptable reproducibility was obtained for analysis of thiophene compounds from spiked seawater samples at RSDs ≤7.0% (n = 3).

  17. Development of a SPME-GC-MS method for the determination of volatile compounds in Shanxi aged vinegar and its analytical characterization by aroma wheel.

    Science.gov (United States)

    Zhu, Hong; Zhu, Jie; Wang, Lili; Li, Zaigui

    2016-01-01

    A solid-phase microextraction followed by gas chromatography-mass spectrometry method was developed to determine the volatile compounds in Shanxi aged vinegar. The optimal extraction conditions were: 50 °C for 20 min with a PDMS/DVB fiber. This analytical method was validated and showed satisfactory repeatability (0.5 %compounds. According to the calculation of odor activity value, 19 volatile compounds were identified as aroma-active compounds. Among them, propanoic acid, acetic acid, trimethyl-oxazole, butanoic acid, acetoin, 3-methylbutanoic acid and furfural were the most powerful odorants. The aroma wheel of Shanxi aged vinegar showed that the classes of sensory descriptors are first fatty and roasty, next woody and nutty and minor fruity and floral. Principal component analysis enabled us to investigate dissimilarity/similarity of Shanxi aged vinegar sample of different raw material and ageing time.

  18. pH-Induced precipitation behavior of weakly basic compounds: determination of extent and duration of supersaturation using potentiometric titration and correlation to solid state properties.

    Science.gov (United States)

    Hsieh, Yi-Ling; Ilevbare, Grace A; Van Eerdenbrugh, Bernard; Box, Karl J; Sanchez-Felix, Manuel Vincente; Taylor, Lynne S

    2012-10-01

    To examine the precipitation and supersaturation behavior of ten weak bases in terms of the relationship between pH-concentration-time profiles and the solid state properties of the precipitated material. Initially the compound was dissolved at low pH, followed by titration with base to induce precipitation. Upon precipitation, small aliquots of acid or base were added to induce slight subsaturation and supersaturation respectively and the resultant pH gradient was determined. The concentration of the unionized species was calculated as a function of time and pH using mass and charge balance equations. Two patterns of behavior were observed in terms of the extent and duration of supersaturation arising following an increase in pH and this behavior could be rationalized based on the crystallization tendency of the compound. For compounds that did not readily crystallize, an amorphous precipitate was formed and a prolonged duration of supersaturation was observed. For compounds that precipitated to crystalline forms, the observed supersaturation was short-lived. This study showed that supersaturation behavior has significant correlation with the solid-state properties of the precipitate and that pH-metric titration methods can be utilized to evaluate the supersaturation behavior.

  19. A Simple and Direct LC-MS Method for Determination of Genotoxic Impurity Hydroxylamine in Pharmaceutical compounds.

    Science.gov (United States)

    Kumar, Thangarathinam; Ramya, Mohandass; Srinivasan, Viswanathan; Xavier, N

    2017-08-01

    Hydroxylamine is a known genotoxic impurity compound that needs to be controlled down to ppm level in pharmaceutical processes. It is difficult to detect using conventional analytical techniques due to its physio-chemical properties like lack of chromophore, low molecular weight, absence of carbon atom and high polarity. In addition to that, analysis of the pharmaceutical samples encounters considerable obstruction from matrix components that greatly overshadow the response of hydroxylamine. This study describes a simple, sensitive and direct Liquid Chromatographic-Mass Spectrometric method (LC-MS) for detection of hydroxylamine in pharmaceutical compounds. The LC-MS method was detected up to 0.008 ppm of hydroxylamine with S/N > 3.0 and quantified up to 0.025 ppm of hydroxylamine with S/N ratio >10.0. This validated method can be applied as a generic method to detect the hydroxylamine for pharmaceutical process control and drug substance release. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  20. A novel amperometric biosensor based on banana peel (Musa cavendish) tissue homogenate for determination of phenolic compounds.

    Science.gov (United States)

    Ozcan, Hakki Mevlut; Sagiroglu, Ayten

    2010-08-01

    In this study the biosensor was constructed by immobilizing tissue homogenate of banana peel onto a glassy carbon electrode surface. Effects of immobilization materials amounts, effects of pH, buffer concentration and temperature on biosensor response were studied. In addition, the detection ranges of 13 phenolic compounds were obtained with the help of the calibration graphs. Storage stability, repeatability of the biosensor, inhibitory effect and sample applications were also investigated. A typical calibration curve for the sensor revealed a linear range of 10-80 microM catechol. In reproducibility studies, variation coefficient and standard deviation were calculated as 2.69%, 1.44 x 10(-3) microM, respectively.

  1. The determination of vitamin C, organic acids, phenolic compounds concentration of Red and Golden delicious apple grown in Lorestan province

    Directory of Open Access Journals (Sweden)

    ebrahim Falahi

    2013-08-01

    Results: Ascorbic acid concentrations in Red and Golden delicious apples were 9.49 and 9.09 mg and 9.29 mg in total per 100 grams. Malic acid concentrations in Red and Golden delicious apples were 0.26 and 0.27 and citric acid concentrations in Red and Golden delicious apples were 0.28 mg per 100 grams in both cultivars. Acidity of Red delicious was 4 and Golden delicious was about 3.7. The acidity of Red delicious was higher than the Golden one. α-farensene was the most phenolic compound in both cultivars. Conclusion: Finally, apple cultivars grown in Lorestan have 3 times more ascorbic acid than the amount which mentioned in Iranian Food Consumption Table. There were no significant relation about malic and citric acid in both cultivars.

  2. The angular structure of ONC201, a TRAIL pathway-inducing compound, determines its potent anti-cancer activity.

    Science.gov (United States)

    Wagner, Jessica; Kline, Christina Leah; Pottorf, Richard S; Nallaganchu, Bhaskara Rao; Olson, Gary L; Dicker, David T; Allen, Joshua E; El-Deiry, Wafik S

    2014-12-30

    We previously identified TRAIL-inducing compound 10 (TIC10), also known as NSC350625 or ONC201, from a NCI chemical library screen as a small molecule that has potent anti-tumor efficacy and a benign safety profile in preclinical cancer models. The chemical structure that was originally published by Stahle, et. al. in the patent literature was described as an imidazo[1,2-a]pyrido[4,3-d]pyrimidine derivative. The NCI and others generally accepted this as the correct structure, which was consistent with the mass spectrometry analysis outlined in the publication by Allen et. al. that first reported the molecule's anticancer properties. A recent publication demonstrated that the chemical structure of ONC201 material from the NCI is an angular [3,4-e] isomer of the originally disclosed, linear [4,3-d] structure. Here we confirm by NMR and X-ray structural analysis of the dihydrochloride salt form that the ONC201 material produced by Oncoceutics is the angular [3,4-e] structure and not the linear structure originally depicted in the patent literature and by the NCI. Similarly, in accordance with our biological evaluation, the previously disclosed anti-cancer activity is associated with the angular structure and not the linear isomer. Together these studies confirm that ONC201, produced by Oncoceutics or obtained from the NCI, possesses an angular [3,4-e] structure that represents the highly active anti-cancer compound utilized in prior preclinical studies and now entering clinical trials in advanced cancers.

  3. Degradation of linear alkylabenzene sulfonate (LAS) and its compounds in Donghu Lake (Hubei, P.R.C.) determined by high performance liquid chromatography (HPLC)

    Science.gov (United States)

    Ayfer, Yediler; Xu, Ying; Zhang, Yongyuan; Chen, Junjian

    1990-06-01

    Commercial linear alkylbenzene sulfonate (LAS), mixture of alkylchain lengths and phenyl position isomers (C10-C13), is widely used as a major constituent of household and industrial detergents in the People's Republic of China. Degradation process and behaviour of LAS compounds during an 82-hour lake water die-away study, with an added LAS concentration of 1.5mg·L-1, was quantified and accomplished by HPLO-UV after extractionon the SepPek C18 reversed-phase cartridges. The degradation rate became progressively faster with increasing chain length. The technique described in this study is fast, sensitive and specific, and can be used to determine low levels of LAS and for establishing water quality criteria and standards relating to LAS and its compounds.

  4. Inductively coupled plasma-mass spectrometry for elemental analysis and isotope ratio determinations in individual organic compounds separated by gas chromatography

    International Nuclear Information System (INIS)

    Chong, N.S.; Houk, R.S.

    1987-01-01

    A gas chromatograph (GC) with a packed column was interfaced to an inductively coupled plasma-mass spectrometer (ICP-MS) to yield atomic mass spectra from volatile organic compounds. Atomization of injected compounds was nearly complete and independent of molecular structure, so that elemental ratios could be determined. Detection limits were in the range 0.001 to 400 ng s -1 , depending on the ionization energy of the element and its abundance in the background spectrum. The relative standard deviation of measured isotope ratios varied from 0.4% for Br (i.e., a ratio close to unity) to 18% for N (a very large ratio). Thus, GC-ICP-MS provides elemental and isotope ratio information that is complementary to the molecular information derived from GC-MS with conventional ionization methods

  5. Biogenic volatile organic compound (BVOC) emissions from forested areas in Turkey: Determination of specific emission rates for thirty-one tree species

    International Nuclear Information System (INIS)

    Aydin, Yagmur Meltem; Yaman, Baris; Koca, Husnu; Dasdemir, Okan; Kara, Melik; Altiok, Hasan; Dumanoglu, Yetkin; Bayram, Abdurrahman; Tolunay, Doganay; Odabasi, Mustafa; Elbir, Tolga

    2014-01-01

    Normalized biogenic volatile organic compound (BVOC) emission rates for thirty one tree species that cover the 98% of national forested areas in Turkey were determined. Field samplings were performed at fourteen different forested areas in Turkey using a specific dynamic enclosure system. The selected branches of tree species were enclosed in a chamber consisted of a transparent Nalofan bag. The air-flows were sampled from both inlet and outlet of the chamber by Tenax-filled sorbent tubes during photosynthesis of trees under the presence of sunlight. Several environmental parameters (temperature, humidity, photosynthetically active radiation-PAR, and CO 2 ) were continuously monitored inside and outside the enclosure chamber during the samplings. Collected samples were analyzed using a gas chromatography mass spectrometry (GC/MS) system equipped with a thermal desorber (TD). Sixty five BVOCs classified in five major groups (isoprene, monoterpenes, sesquiterpenes, oxygenated sesquiterpenes, and other oxygenated compounds) were analyzed. Emission rates were determined by normalization to standard conditions (1000 μmol/m 2 s PAR and 30 °C temperature for isoprene and 30 °C temperature for the remaining compounds). In agreement with the literature, isoprene was mostly emitted by broad-leaved trees while coniferous species mainly emitted monoterpenes. Several tree species such as Sweet Chestnut, Silver Lime, and European Alder had higher monoterpene emissions although they are broad-leaved species. High isoprene emissions were also observed for a few coniferous species such as Nordmann Fir and Oriental Spruce. The highest normalized total BVOC emission rate of 27.1 μg/g h was observed for Oriental Plane while South European Flowering Ash was the weakest BVOC emitter with a total normalized emission rate of 0.031 μg/g h. Monoterpene emissions of broad-leaved species mainly consisted of sabinene, limonene and trans-beta-ocimene, while alpha-pinene, beta-pinene and

  6. Biogenic volatile organic compound (BVOC) emissions from forested areas in Turkey: Determination of specific emission rates for thirty-one tree species

    Energy Technology Data Exchange (ETDEWEB)

    Aydin, Yagmur Meltem; Yaman, Baris; Koca, Husnu; Dasdemir, Okan; Kara, Melik; Altiok, Hasan; Dumanoglu, Yetkin; Bayram, Abdurrahman [Department of Environmental Engineering, Faculty of Engineering, Dokuz Eylul University, Tinaztepe Campus, Buca, Izmir (Turkey); Tolunay, Doganay [Department of Soil Science and Ecology, Faculty of Forestry, Istanbul University, Bahcekoy, Istanbul (Turkey); Odabasi, Mustafa [Department of Environmental Engineering, Faculty of Engineering, Dokuz Eylul University, Tinaztepe Campus, Buca, Izmir (Turkey); Elbir, Tolga, E-mail: tolga.elbir@deu.edu.tr [Department of Environmental Engineering, Faculty of Engineering, Dokuz Eylul University, Tinaztepe Campus, Buca, Izmir (Turkey)

    2014-08-15

    Normalized biogenic volatile organic compound (BVOC) emission rates for thirty one tree species that cover the 98% of national forested areas in Turkey were determined. Field samplings were performed at fourteen different forested areas in Turkey using a specific dynamic enclosure system. The selected branches of tree species were enclosed in a chamber consisted of a transparent Nalofan bag. The air-flows were sampled from both inlet and outlet of the chamber by Tenax-filled sorbent tubes during photosynthesis of trees under the presence of sunlight. Several environmental parameters (temperature, humidity, photosynthetically active radiation-PAR, and CO{sub 2}) were continuously monitored inside and outside the enclosure chamber during the samplings. Collected samples were analyzed using a gas chromatography mass spectrometry (GC/MS) system equipped with a thermal desorber (TD). Sixty five BVOCs classified in five major groups (isoprene, monoterpenes, sesquiterpenes, oxygenated sesquiterpenes, and other oxygenated compounds) were analyzed. Emission rates were determined by normalization to standard conditions (1000 μmol/m{sup 2} s PAR and 30 °C temperature for isoprene and 30 °C temperature for the remaining compounds). In agreement with the literature, isoprene was mostly emitted by broad-leaved trees while coniferous species mainly emitted monoterpenes. Several tree species such as Sweet Chestnut, Silver Lime, and European Alder had higher monoterpene emissions although they are broad-leaved species. High isoprene emissions were also observed for a few coniferous species such as Nordmann Fir and Oriental Spruce. The highest normalized total BVOC emission rate of 27.1 μg/g h was observed for Oriental Plane while South European Flowering Ash was the weakest BVOC emitter with a total normalized emission rate of 0.031 μg/g h. Monoterpene emissions of broad-leaved species mainly consisted of sabinene, limonene and trans-beta-ocimene, while alpha-pinene, beta

  7. [Chromatographic mass spectrometric determination of low-molecular-weight aromatic compounds of microbial origin in the serum from patients with sepsis].

    Science.gov (United States)

    Beloborodova, N V; Arkhipova, A S; Beloborodov, D M; Boĭko, N B; Mel'ko, A I; Olenin, A Iu

    2006-02-01

    The investigation quantitatively determined the content of low-molecular-weight aromatic compounds of microbial origin in the sera of 34 individuals by chromatographic mass spectrometry. An "Agilent Technogies 6890N" gas chromatograph with a 5973 mass selective detector was applied; chromatographic separation of components was effected on an Hp-5MS quartz capillary column. Aromatic small molecules originating from microbes (SMOM) were determined in the sera of 7 patients with sepsis. The diagnosis of sepsis was documented by the presence of the systemic inflammation syndrome and by that of bacteriemia and/or artificial ventilation-associated pneumonia along with the level of procalcitonin of higher than 10 ng/ml. The levels of aromatic SMOM were compared in 10 healthy donors, 8 preoperative cardiosurgical patients, and 9 patients with different abnormalities without sepsis treated in an intensive care unit (ICU). Serum phenylacetic and 3-phenylpropionic acids were found to be prevalent in the healthy donors and postoperative cardiosurgical patients. In ICU patients with different complications without sepsis, more than half the compounds under study were undetectable, the others were found in very low concentrations, which may be accounted for by antibiotic therapy. At the same time, almost the whole spectrum of the test compounds (other than 3-phenylpropionic acid) with the highest concentrations of 3-phenyllactic, p-hydroxyphenylacetic, 3-(p-hydroxyphenyl)lactic and 2-hydroxybutanic acids, was detectable in septic patients receiving a more intensive therapy. The differences were statistically significant (by the Mann-Whitney U-test; p < 0.05). By taking into account the potentially high biological activity of the test compounds, studies are to be continued in this area.

  8. Occurrence of different classes of perfluorinated compounds in Greek wastewater treatment plants and determination of their solid–water distribution coefficients

    International Nuclear Information System (INIS)

    Arvaniti, Olga S.; Ventouri, Elpida I.; Stasinakis, Athanasios S.; Thomaidis, Nikolaos S.

    2012-01-01

    Highlights: ► Eighteen PFCs were determined in wastewater and sludge samples using LC–MS/MS. ► PFPeA, PFOA and PFOS were the dominating compounds in both WWTPs. ► No significant decrease or even increase of most PFCs was noticed in effluents. ► Distribution coefficients of PFCs were calculated for different types of sludge. ► Sorption potential was affected by the target compound and the type of sludge. - Abstract: The concentrations of eighteen perfluorinated compounds (PFCs: C5–C14 carboxylates, C4, C6–C8 and C10 sulfonates and 3 sulfonamides) were determined in wastewater and sludge samples originating from two different wastewater treatment plants (WWTPs). The analytes were extracted by solid phase extraction (dissolved phase) or sonication followed by solid phase extraction (solid phase). Qualitative and quantitative analyses were performed by LC–MS/MS. According to the results, perfluoropentanoic acid (PFPeA), perfluorooctanoic acid (PFOA) and perfluorooctane sulfonate (PFOS) were dominant in wastewater and sludge samples from both plants. The average concentrations in the raw and treated wastewater ranged up to 75.7 ng L −1 (perfluorotridecanoic acid, PFTrDA) and 76.0 ng L −1 (PFPeA), respectively. Concentrations of most PFCs were higher in effluents than in influents, indicating their formation during wastewater treatment processes. In sewage sludge, the average concentrations ranged up to 6.7 ng g −1 dry weight (PFOS). No significant seasonal variations in PFCs concentrations were observed, while higher concentrations of PFOA, PFOS and perfluorononanoic acid (PFNA) were determined in the WWTP receiving municipal and industrial wastewater. Significantly different distribution coefficient (K d ) values were determined for different PFCs and different type of sludge, ranging between 169 L kg −1 (PFHxS) to 12,922 L kg −1 (PFDA).

  9. The determination of small amounts of fluoride in uranium compounds by use of an ion-selective electrode

    International Nuclear Information System (INIS)

    Shelton, B.M.

    1975-01-01

    A method is presented for the determination of fluoride in uranium metal and oxide at levels from 16 p.p.m. upwards. Uranium is separated from fluoride by extraction into a solution of di(2-ethylhexyl)-phosphoric acid (HDEHP) in carbon tetrachloride. The fluoride remaining in the aqueous phase is determined by potentiometric measurement with an ion-selective electrode. A correction is made for the fluoride lost during the dissolution or extraction step, or both, which is based on a determination of the apparent loss of fluoride on spiked samples that are taken through the whole procedure [af

  10. Determination of Partition coefficients for a Mixture of Volatile Organic Compounds in Rats and Humans at Different Life Stages

    National Research Council Canada - National Science Library

    Mahle, Deidre A; Gearhart, Jeffrey M; Godfrey, Richard J; Mattie, David R; Cook, Robert S; Grisby, Claude C

    2004-01-01

    .... Partition coefficients (PCs) are an integral component of pharmacokinetic models and determining differences in tissue partitioning of volatile organic chemicals across life stages can help reduce the uncertainty in risk assessment...

  11. A Field Method For Determination of Groundwater and Groundwater-sediment Associated Potentials for Degradation of Xenobiotic Organic Compounds

    DEFF Research Database (Denmark)

    Nielsen, Per Henning; Christensen, Thomas Højlund; Holm, Peter Engelund

    1992-01-01

    Determination of the degradation potentials for a mixture of eight organic trace contaminants (benzene, toluene, o-xylene, naphthalene, tetrachloromethane, 1,1,1-trichloroethane, trichloroethene, tetrachloroethene) has been made by specially developed in situ microcosms under aerobic and anaerobi...

  12. Determination of n-octanol/water partition coefficient for DDT-related compounds by RP-HPLC with a novel dual-point retention time correction.

    Science.gov (United States)

    Han, Shu-ying; Qiao, Jun-qin; Zhang, Yun-yang; Yang, Li-li; Lian, Hong-zhen; Ge, Xin; Chen, Hong-yuan

    2011-03-01

    n-Octanol/water partition coefficients (P) for DDTs and dicofol were determined by reversed-phase high performance liquid chromatography (RP-HPLC) on a C(18) column using methanol-water mixture as mobile phase. A dual-point retention time correction (DP-RTC) was proposed to rectify chromatographic retention time (t(R)) shift resulted from stationary phase aging. Based on this correction, the relationship between logP and logk(w), the logarithm of the retention factor extrapolated to pure water, was investigated for a set of 12 benzene homologues and DDT-related compounds with reliable experimental P as model compounds. A linear regression logP=(1.10±0.04) logk(w) - (0.60±0.17) was established with correlation coefficient R(2) of 0.988, cross-validated correlation coefficient R(cv)(2) of 0.983 and standard deviation (SD) of 0.156. This model was further validated using four verification compounds, naphthalene, biphenyl, 2,2-bis(4-chlorophenyl)-1,1-dichloroethane (p,p'-DDD) and 2,2-bis(4-chlorophenyl)-1,1-dichloroethene (p,p'-DDE) with similar structure to DDT. The RP-HPLC-determined P values showed good consistency with shake-flask (SFM) or slow-stirring (SSM) results, especially for highly hydrophobic compounds with logP in the range of 4-7. Then, the P values for five DDT-related compounds, 2-(2-chlorophenyl)-2-(4-chlorophenyl)-1,1,1-trichloroethane (o,p'-DDT), 2-(2-chlorophenyl)-2-(4-chlorophenyl)-1,1-dichloroethane (o,p'-DDD), 2-(2-chlorophenyl)-2-(4-chlorophenyl)-1,1-dichloroethene (o,p'-DDE), and 2,2,2-trichloro-1,1-bis(4-chlorophenyl)ethanol (dicofol) and its main degradation product 4,4'-dichlorobenzophenone (p,p'-DBP) were evaluated by the improved RP-HPLC method for the first time. The excellent precision with SD less than 0.03 proved that the novel DP-RTC protocol can significantly increases the determination accuracy and reliability of P by RP-HPLC. Copyright © 2011 Elsevier Ltd. All rights reserved.

  13. Determination of volatile organic compounds in water by headspace solid-phase microextraction gas chromatography coupled to tandem mass spectrometry with triple quadrupole analyzer

    International Nuclear Information System (INIS)

    Cervera, M.I.; Beltran, J.; Lopez, F.J.; Hernandez, F.

    2011-01-01

    Highlights: → Employing a statistical optimization improves results reducing experiments. → Use of MS (QqQ) allows high sensitivity determination and improves identification capabilities. → Using Q/q intensity ratios is a powerful tool to ensure compound identification. → HS SPME GC-MS/MS method allows determination of VOCs in complex matrix water samples. - Abstract: In the present work, a rapid method with little sample handling has been developed for determination of 23 selected volatile organic compounds in environmental and wastewater samples. The method is based on headspace solid-phase microextraction (SPME) followed by gas chromatography coupled to tandem mass spectrometry (GC-MS/MS) determination using triple quadrupole analyzer (QqQ) in electron ionization mode. The best conditions for extraction were optimised with a factorial design taking into account the interaction between different parameters and not only individual effects of variables. In the optimized procedure, 4 mL of water sample were extracted using a 10 mL vial and adding 0.4 g NaCl (final NaCl content of 10%). An SPME extraction with carboxen/polydimethylsiloxane 75 μm fiber for 30 min at 50 deg. C (with 5 min of previous equilibration time) with magnetic stirring was applied. Chromatographic determination was carried out by GC-MS/MS working in Selected Reaction Monitoring (SRM) mode. For most analytes, two MS/MS transitions were acquired, although for a few compounds it was difficult to obtain characteristic abundant fragments. In those cases, a pseudo selected reaction monitoring (pseudo-SRM) with three ions was used instead. The intensity ratio between quantitation (Q) and confirmation (q) signals was used as a confirmatory parameter. The method was validated by means of recovery experiments (n = 6) spiking mineral water samples at three concentration levels (0.1, 5 and 50 μg L -1 ). Recoveries between 70% and 120% were generally obtained with relative standard deviations (RSDs

  14. Determination of volatile organic compounds in water by headspace solid-phase microextraction gas chromatography coupled to tandem mass spectrometry with triple quadrupole analyzer

    Energy Technology Data Exchange (ETDEWEB)

    Cervera, M.I. [Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat, E-12071 Castellon (Spain); Beltran, J., E-mail: joaquim.beltran@uji.es [Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat, E-12071 Castellon (Spain); Lopez, F.J.; Hernandez, F. [Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat, E-12071 Castellon (Spain)

    2011-10-17

    Highlights: {yields} Employing a statistical optimization improves results reducing experiments. {yields} Use of MS (QqQ) allows high sensitivity determination and improves identification capabilities. {yields} Using Q/q intensity ratios is a powerful tool to ensure compound identification. {yields} HS SPME GC-MS/MS method allows determination of VOCs in complex matrix water samples. - Abstract: In the present work, a rapid method with little sample handling has been developed for determination of 23 selected volatile organic compounds in environmental and wastewater samples. The method is based on headspace solid-phase microextraction (SPME) followed by gas chromatography coupled to tandem mass spectrometry (GC-MS/MS) determination using triple quadrupole analyzer (QqQ) in electron ionization mode. The best conditions for extraction were optimised with a factorial design taking into account the interaction between different parameters and not only individual effects of variables. In the optimized procedure, 4 mL of water sample were extracted using a 10 mL vial and adding 0.4 g NaCl (final NaCl content of 10%). An SPME extraction with carboxen/polydimethylsiloxane 75 {mu}m fiber for 30 min at 50 deg. C (with 5 min of previous equilibration time) with magnetic stirring was applied. Chromatographic determination was carried out by GC-MS/MS working in Selected Reaction Monitoring (SRM) mode. For most analytes, two MS/MS transitions were acquired, although for a few compounds it was difficult to obtain characteristic abundant fragments. In those cases, a pseudo selected reaction monitoring (pseudo-SRM) with three ions was used instead. The intensity ratio between quantitation (Q) and confirmation (q) signals was used as a confirmatory parameter. The method was validated by means of recovery experiments (n = 6) spiking mineral water samples at three concentration levels (0.1, 5 and 50 {mu}g L{sup -1}). Recoveries between 70% and 120% were generally obtained with

  15. A dynamic dilution system-based evaluation of the procedure adopted for determining ozone precursor volatile compounds.

    Science.gov (United States)

    Palluau, Fabienne; Mirabel, Philippe; Millet, Maurice

    2005-02-01

    A dynamic dilution system was created to evaluate the performance and the reliability of ozone precursor volatile organic compound (VOC) sampling ("TO-Can" canisters) and analysis (thermal desorption/gas chromatography/flame ionisation detection) techniques used by the "Laboratoire Interregional de Chimie du Grand Est (LIC)". Different atmospheres of VOCs were generated at concentrations between 0.8 and 25 ppb, with temperatures of 0, 10, 20 and 30 degrees C, and with relative humidities of 0, 30, 50, 70 and 90%. These conditions are generally representative of those commonly observed in ambient air in the eastern France. This dynamic dilution allows the simulation of a wide range of scenarios (concentrations, temperatures and relative humidities). After assessing the capacity and performance of the system, it was applied in order to evaluate the recoveries and stabilities of VOCs from canisters used for the collection and analysis of two mixtures of VOCs. The first mixture contained six alkanes (ethane, propane, butane, pentane, hexane and heptane), and the second contained five alkenes (ethene, propene, butene, 1-pentene and 1-hexene), five aromatics (benzene, toluene, ethylbenzene, m-xylene and o-xylene), acetylene, and 1,3-butadiene. No significant losses of alkanes from the canisters were observed after 21 days of storage, and good recoveries of alkanes from the canisters (>80%) were obtained regardless of the concentration, the temperature and the relative humidity. However, losses of certain aromatics were noted at low relative humidity.

  16. Rapid determination of floral aroma compounds of lilac blossom by fast gas chromatography combined with surface acoustic wave sensor.

    Science.gov (United States)

    Oh, Se Yeon; Shin, Hyun Du; Kim, Sung Jean; Hong, Jongki

    2008-03-07

    A novel analytical method using fast gas chromatography combined with surface acoustic wave sensor (GC/SAW) has been developed for the detection of volatile aroma compounds emanated from lilac blossom (Syringa species: Syringa vulgaris variginata and Syringa dilatata). GC/SAW could detect and quantify various fragrance emitted from lilac blossom, enabling to provide fragrance pattern analysis results. The fragrance pattern analysis could easily characterize the delicate differences in aromas caused by the substantial difference of chemical composition according to different color and shape of petals. Moreover, the method validation of GC/SAW was performed for the purpose of volatile floral actual aroma analysis, achieving a high reproducibility and excellent sensitivity. From the validation results, GC/SAW could serve as an alternative analytical technique for the analysis of volatile floral actual aroma of lilac. In addition, headspace solid-phase microextraction (HS-SPME) GC-MS was employed to further confirm the identification of fragrances emitted from lilac blossom and compared to GC/SAW.

  17. Determination of perfluorinated compounds in fish fillet homogenates: method validation and application to fillet homogenates from the Mississippi River.

    Science.gov (United States)

    Malinsky, Michelle Duval; Jacoby, Cliffton B; Reagen, William K

    2011-01-10

    We report herein a simple protein precipitation extraction-liquid chromatography tandem mass spectrometry (LC/MS/MS) method, validation, and application for the analysis of perfluorinated carboxylic acids (C7-C12), perfluorinated sulfonic acids (C4, C6, and C8), and perfluorooctane sulfonamide (FOSA) in fish fillet tissue. The method combines a rapid homogenization and protein precipitation tissue extraction procedure using stable-isotope internal standard (IS) calibration. Method validation in bluegill (Lepomis macrochirus) fillet tissue evaluated the following: (1) method accuracy and precision in both extracted matrix-matched calibration and solvent (unextracted) calibration, (2) quantitation of mixed branched and linear isomers of perfluorooctanoate (PFOA) and perfluorooctanesulfonate (PFOS) with linear isomer calibration, (3) quantitation of low level (ppb) perfluorinated compounds (PFCs) in the presence of high level (ppm) PFOS, and (4) specificity from matrix interferences. Both calibration techniques produced method accuracy of at least 100±13% with a precision (%RSD) ≤18% for all target analytes. Method accuracy and precision results for fillet samples from nine different fish species taken from the Mississippi River in 2008 and 2009 are also presented. Copyright © 2010 Elsevier B.V. All rights reserved.

  18. Determination of perfluorinated compounds in fish fillet homogenates: Method validation and application to fillet homogenates from the Mississippi River

    International Nuclear Information System (INIS)

    Malinsky, Michelle Duval; Jacoby, Cliffton B.; Reagen, William K.

    2011-01-01

    We report herein a simple protein precipitation extraction-liquid chromatography tandem mass spectrometry (LC/MS/MS) method, validation, and application for the analysis of perfluorinated carboxylic acids (C7-C12), perfluorinated sulfonic acids (C4, C6, and C8), and perfluorooctane sulfonamide (FOSA) in fish fillet tissue. The method combines a rapid homogenization and protein precipitation tissue extraction procedure using stable-isotope internal standard (IS) calibration. Method validation in bluegill (Lepomis macrochirus) fillet tissue evaluated the following: (1) method accuracy and precision in both extracted matrix-matched calibration and solvent (unextracted) calibration, (2) quantitation of mixed branched and linear isomers of perfluorooctanoate (PFOA) and perfluorooctanesulfonate (PFOS) with linear isomer calibration, (3) quantitation of low level (ppb) perfluorinated compounds (PFCs) in the presence of high level (ppm) PFOS, and (4) specificity from matrix interferences. Both calibration techniques produced method accuracy of at least 100 ± 13% with a precision (%RSD) ≤18% for all target analytes. Method accuracy and precision results for fillet samples from nine different fish species taken from the Mississippi River in 2008 and 2009 are also presented.

  19. Determination of perfluorinated compounds in fish fillet homogenates: Method validation and application to fillet homogenates from the Mississippi River

    Energy Technology Data Exchange (ETDEWEB)

    Malinsky, Michelle Duval, E-mail: mmalinsky@mmm.com [3M Environmental Laboratory, 3M Center, Building 0260-05-N-17, St. Paul, MN 55144-1000 (United States); Jacoby, Cliffton B.; Reagen, William K. [3M Environmental Laboratory, 3M Center, Building 0260-05-N-17, St. Paul, MN 55144-1000 (United States)

    2011-01-10

    We report herein a simple protein precipitation extraction-liquid chromatography tandem mass spectrometry (LC/MS/MS) method, validation, and application for the analysis of perfluorinated carboxylic acids (C7-C12), perfluorinated sulfonic acids (C4, C6, and C8), and perfluorooctane sulfonamide (FOSA) in fish fillet tissue. The method combines a rapid homogenization and protein precipitation tissue extraction procedure using stable-isotope internal standard (IS) calibration. Method validation in bluegill (Lepomis macrochirus) fillet tissue evaluated the following: (1) method accuracy and precision in both extracted matrix-matched calibration and solvent (unextracted) calibration, (2) quantitation of mixed branched and linear isomers of perfluorooctanoate (PFOA) and perfluorooctanesulfonate (PFOS) with linear isomer calibration, (3) quantitation of low level (ppb) perfluorinated compounds (PFCs) in the presence of high level (ppm) PFOS, and (4) specificity from matrix interferences. Both calibration techniques produced method accuracy of at least 100 {+-} 13% with a precision (%RSD) {<=}18% for all target analytes. Method accuracy and precision results for fillet samples from nine different fish species taken from the Mississippi River in 2008 and 2009 are also presented.

  20. Application of self-organising maps towards segmentation of soybean samples by determination of inorganic compounds content.

    Science.gov (United States)

    Cremasco, Hágata; Borsato, Dionísio; Angilelli, Karina Gomes; Galão, Olívio Fernandes; Bona, Evandro; Valle, Marcos Eduardo

    2016-01-15

    In this study, 20 samples of soybean, both transgenic and conventional cultivars, which were planted in two different regions, Londrina and Ponta Grossa, both located at Paraná, Brazil, were analysed. In order to verify whether the inorganic compound levels in soybeans varied with the region of planting, K, P, Ca, Mg, S, Zn, Mn, Fe, Cu and B contents were analysed by an artificial neural network self-organising map. It was observed that with a topology 10 × 10, 8000 epochs, initial learning rate of 0.1 and initial neighbourhood ratio of 4.5, the network was able to differentiate samples according to region of origin. Among all of the variables analysed by the artificial neural network, the elements Zn, Ca and Mn were those which most contributed to the classification of the samples. The results indicated that samples planted in these two regions differ in their mineral content; however, conventional and transgenic samples grown in the same region show no difference in mineral contents in the grain. © 2015 Society of Chemical Industry.

  1. Determination of phosphate compounds in meat products by 31-Phosphorus Nuclear Magnetic Resonance spectroscopy with methylenediphosphonic acid after alkaline extraction

    International Nuclear Information System (INIS)

    Hrynczyszyn, P.; Jastrzebska, A.; Szlyk, E.

    2010-01-01

    Modification of the extraction procedure and application of the 31 P NMR method for the determination of polyphosphates in meat products were studied. In the elaborated procedure threefold water extraction at alkaline pH (borate buffer and 0.1 M EDTA) was applied. Furthermore, the new external standard for 31 P NMR determination of phosphates was proposed. Obtained recoveries were between 95 and 99% and variation coefficients (CV) was ≤5%, indicating an increase in accuracy and the precision of the proposed procedure in relation to the spectrophotometric method. The described procedure of sample preparation with 31 P NMR method was applied for the determination of polyphosphate additives in meat products. The satisfactory precision (CV = 0.39-3.40%) shows the benefit of the NMR method in the routine analysis of the phosphate ions in meat products.

  2. Enantiomeric determination of amino compounds with high sensitivity using the chiral reagents (+)- and (-)-1-(9-anthryl)-2-propyl chloroformate.

    Science.gov (United States)

    Thorsén, G; Engström, A; Josefsson, B

    1997-10-31

    New chiral precolumn reagents, (+)- and (-)-1-(9-anthryl)-2-propyl chloroformate (APOC), are introduced for the chiral separation of amino acids and small peptides in capillary electrophoresis. Chiral separation of 17 amino acids and four small peptides as their diastereomeric 1-(9-anthryl)-2-propyl carbamate derivatives have been achieved by micellar electrokinetic chromatography. The detection limit for the derivatives is in the femtomole range with UV detection and in the attomole range with laser-induced fluorescence (LIF) detection. LIF detection was used to determine the enantiomeric excess of four APOC-derivatised peptides. The use of the new, anthracene-based reagents in conjunction with argon ion LIF makes enantiomeric determinations at ppm levels feasible. In this paper determinations below promille levels are performed without overloading the separation system.

  3. Determination of reversed-phase high performance liquid chromatography based octanol-water partition coefficients for neutral and ionizable compounds: Methodology evaluation.

    Science.gov (United States)

    Liang, Chao; Qiao, Jun-Qin; Lian, Hong-Zhen

    2017-12-15

    Reversed-phase liquid chromatography (RPLC) based octanol-water partition coefficient (logP) or distribution coefficient (logD) determination methods were revisited and assessed comprehensively. Classic isocratic and some gradient RPLC methods were conducted and evaluated for neutral, weak acid and basic compounds. Different lipophilicity indexes in logP or logD determination were discussed in detail, including the retention factor logk w corresponding to neat water as mobile phase extrapolated via linear solvent strength (LSS) model from isocratic runs and calculated with software from gradient runs, the chromatographic hydrophobicity index (CHI), apparent gradient capacity factor (k g ') and gradient retention time (t g ). Among the lipophilicity indexes discussed, logk w from whether isocratic or gradient elution methods best correlated with logP or logD. Therefore logk w is recommended as the preferred lipophilicity index for logP or logD determination. logk w easily calculated from methanol gradient runs might be the main candidate to replace logk w calculated from classic isocratic run as the ideal lipophilicity index. These revisited RPLC methods were not applicable for strongly ionized compounds that are hardly ion-suppressed. A previously reported imperfect ion-pair RPLC method was attempted and further explored for studying distribution coefficients (logD) of sulfonic acids that totally ionized in the mobile phase. Notably, experimental logD values of sulfonic acids were given for the first time. The IP-RPLC method provided a distinct way to explore logD values of ionized compounds. Copyright © 2017 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2014-11-01

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

  5. Determination of the major compounds in the extract of the subterranean termite Macrotermes gilvus Hagen digestive tract by GC-MS method

    Directory of Open Access Journals (Sweden)

    N. Subekti

    2017-08-01

    Full Text Available Degradation of woody components by termites is associated with symbionts inside their digestive tract. In this study, the major compounds were determined in the extract of the termite guts by GC-MS method. Macrotermes gilvus Hagen (worker caste termites were collected and their dissected guts underwent methanol extraction. It was found that the gut of the termites has an alkaline environment (pH 8.83 ± 0.31 that supports the digestion of lignocellulose biomass and also helps to solubilize phenolic and recalcitrant compounds resul­ting from the depolymerization of woody components. The GC-MS analysis showed that termite guts contained hydrophobic organosilicon components including dodecamethylcyclohexasiloxane, tetradecamethylcyclohexa­siloxane, hexadecamethylcyclooctasiloxane, and octasiloxane, 1,1,3,3,5,5,7,7,9,9,11,11,13,13,15,15-hexa­decamethyl. The guts also contained a phytosterol, which was identified as β-sitosterol. Further analysis of these water-insoluble compounds is needed to reveal their importance in termite digestion.

  6. Headspace solid-phase microextraction for the determination of volatile organic sulphur and selenium compounds in beers, wines and spirits using gas chromatography and atomic emission detection.

    Science.gov (United States)

    Campillo, Natalia; Peñalver, Rosa; López-García, Ignacio; Hernández-Córdoba, Manuel

    2009-09-25

    A rapid and solvent-free method for the determination of eight volatile organic sulphur and two selenium compounds in different beverage samples using headspace solid-phase microextraction and gas chromatography with atomic emission detection has been developed. The bonded carboxen/polydimethylsiloxane fiber was the most suitable for preconcentrating the analytes from the headspace of the sample solution. Volumes of 20 mL of undiluted beer were used while, in the case of wines and spirits, sample:water ratios of 5:15 and 2:18, respectively, were used, in order to obtain the maximum sensitivity. Quantitation was carried out by using synthetic matrices of beer and wine, and a spiked sample for spirits, and using ethyl methyl sulphide and isopropyl disulphide as internal standards. Detection limits ranged from 8 ng L(-1) to 40 ng mL(-1), depending on the compound and the beverage sample analyzed, with a fiber time exposure of 20 min at ambient temperature. The optimized method was successfully applied to different samples, some of the studied compounds being detected at concentration levels in the 0.04-152 ng mL(-1) range.

  7. Trace-level determination of polar flavour compounds in butter by solid-phase extraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Adahchour, M; Vreuls, R J; van der Heijden, A; Brinkman, U A

    1999-06-04

    Volatile compounds are responsible for the aromas of butter. A simple technique for the determination of these components is described which is based on solid-phase extraction (SPE) after melting of the butter and separation of the aqueous phase from the fat. Volatile flavours present in the water fraction are collected by off-line SPE on cartidges packed with a copolymer sorbent. After desorption with 500 microliters of methyl acetate, 1-microliter aliquots are quantified and/or identified by gas chromatography-mass spectrometry. The procedure was tested with respect to recovery, linearity and limit of detection in real-life samples using five polar model analytes. It allows the characterisation of polar flavour compounds in butter prior to and after heat treatment at 170 degrees C. From the five model compounds, vanillin, traces of diacetyl and maltol were found to be present in the butter samples. After heat treatment 500-1000-fold increased concentration of maltol, and substantial amounts of furaneol were detected.

  8. Simultaneous Determination of Nine Active Compounds of the Traditional Chinese Medicinal Prescription Shaoyao-Gancao-Tang and Analysis of the Relationship between Therapeutical Effect and Compatibility of Medicines

    Science.gov (United States)

    Zhang, Guijun; Wang, Meng; Wang, Jingjuan; Zeng, Weixin; Gao, Xiaomei

    2014-01-01

    A simple and sensitive HPLC-DAD detection method was established for the simultaneous determination of nine compounds including oxypaeoniflorin, albiflorin, paeoniflorin, benzoylpaeoniflorin, glycyrrhizic acid, liquiritin, isoliquiritin, liquiritigenin, and isoliquiritigenin in the Traditional Chinese Medicinal Prescription Shaoyao-Gancao-Tang (SGT) and we analyze the relationship between therapeutical effect and compatibility of medicines by using an Agilent extend-C18 column at a flow rate of 1 mL/min. The column temperature was maintained at 30°C and the detection wavelength was set at 230 nm for oxypaeoniflorin, albiflorin, paeoniflorin, benzoylpaeoniflorin, and glycyrrhizic acid; 276 nm for liquiritin and liquiritigenin; 360 nm for isoliquiritin and isoliquiritigenin. The total contents of the nine compounds in SGT varied from 4.65 to 20.06 mg/mL. The results of this study showed that the content of chemical compounds of Traditional Chinese Medicinal Prescription is mainly influenced by the dosage and compatibility of medicines and the therapeutical effect of Traditional Chinese Medicinal prescription is mainly influenced by the dosage and compatibility of medicines. The method could be suitable for quality control of SGT with bioactive multicompounds. PMID:25431610

  9. Development of a fast liquid chromatography-tandem mass spectrometry method for the determination of endocrine-disrupting compounds in waters.

    Science.gov (United States)

    Di Carro, Marina; Scapolla, Carlo; Liscio, Camilla; Magi, Emanuele

    2010-09-01

    A fast liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS-MS) method was developed to study five endocrine-disrupting compounds (4-n-nonylphenol, bisphenol A, estrone, 17β-estradiol and 17α-ethinylestradiol) in water. Different columns were tested; the chromatographic separation of the analytes was optimized on a Pinnacle DB biphenylic column with a water-acetonitrile gradient elution, which allowed the separation of the selected endocrine-disrupting compounds (EDCs) in less than 6 min. Quantitative analysis was performed in selected reaction monitoring (SRM) mode; two transitions were chosen for each compound, using the most abundant for quantitation. Calibration curves using bisphenol A-d (16) as internal standard were drawn, showing good correlation coefficients (0.9993-0.9998). All figures of merit of the method were satisfactory; limits of detection were in the low pg range for all analytes. The method was then applied to the determination of the analytes in real water samples: to this aim, polar organic chemical integrative samplers (POCIS) were deployed in the influent and in the effluent of a drinking water treatment plant in Liguria (Italy). The EDC level was rather low in the influent and negligible in the outlet, reflecting the expected function of the treatment plant.

  10. World-wide and regional intercomparison for the determination of organochlorine compounds and petroleum hydrocarbons in mussel sample IAEA-142. Report no. 59

    International Nuclear Information System (INIS)

    Villeneuve, J.P.; Horvat, M.; Cattini, C.

    1996-03-01

    The accurate and precise determination of organochlorine compounds and petroleum hydrocarbons in marine environmental samples is an important aspect of marine pollution assessments in coastal and ocean environments. Intercomparison exercises represent an essential element of method testing and are used as a basic tool for evaluating data quality on a global and regional level. The Marine Environmental Studies Laboratory (MESL) of IAEA-MEL has conducted intercomparison exercises on trace organic compounds for over nineteen years as part of its contribution to IAEA's analytical quality control service and UNEP's regional seas programme, and occasionally in association with the intergovernmental oceanographic commission (of UNESCO) GIPME programme. These exercises are organized on a continuous basis, at least once per year. Result of previous exercises have revealed serious problems for many regional laboratories to obtain comparable data. As a consequence of this situation, it was decided to seek increased support for quality assurance programmes. Staff of MESL, with funding from UNEP, the World Bank and regional trust funds, embarked on a campaign to train analysts in modern measurement techniques, supply appropriate and reliable reference methods and materials and, where possible, to improve analytical instruments in Member State laboratories. This report describes results of the IAEA/UNEP intercomparison run 142 for the chemical analysis of organochlorine compounds and petroleum hydrocarbons in a homogenised mussel sample

  11. Rapid determination of the aromatic compounds methyl-anthranilate, 2'-aminoacetophenone and furaneol by GC-MS: Method validation and characterization of grape derivatives.

    Science.gov (United States)

    Prudêncio Dutra, Maria da Conceição; de Souza, Joyce Fagundes; Viana, Arão Cardoso; de Oliveira, Débora; Pereira, Giuliano Elias; Dos Santos Lima, Marcos

    2018-05-01

    A methodology for the rapid determination of the aromatic compounds methyl anthranilate (MA), 2'-aminoacetophenone (2-AAP) and furaneol by GC-MS was validated and used to characterize grape juice and wine elaborated with the new Brazilian grape varieties cultivated in northeastern Brazil, and Brazilian grape nectars. The method presented linearity (R 2  ˃ 0.9952), good accuracy (CV furaneol in the aroma of grape juice and wines elaborated with the new Brazilian grape varieties. Copyright © 2018 Elsevier Ltd. All rights reserved.

  12. The use of Sphagnum recurvum Pal. Beauv. as biological tests for determination of the level of pollution with fluorine compounds and sulphur dioxide in the environment

    Directory of Open Access Journals (Sweden)

    Maria Świeboda

    2014-01-01

    Full Text Available The green parts of the peat moss Sphagnum recurvum Pal. Beauv. were used as a biological test to evaluate the pollution level of the natural environment in the region of the aluminium works "Skawina" (Southern Poland with fluorine compounds and sulphur dioxide. The moss samples were placed in nylon nets and exposed to the polluted air for 6 weeks, then the fluorine and sulphur content in them was determined. The results demonstrated the usefulness of this method for the purpose of establishing the range of influence of the emitted industrial pollution.

  13. Determination of oxygen in uranium compounds using sulfur monochloride; Dosage de l'oxygene dans les composes de l'uranium par la methode au monochlorure de soufre

    Energy Technology Data Exchange (ETDEWEB)

    Baudin, G; Besson, J; Blum, P L; Tran-Van, Danh [Commisariat a l' Energie Atomique, Grenoble (France). Centre d' Etudes Nucleaires

    1964-07-01

    The authors have described in an other paper (Anal. Chim. Acta, in press) a method for oxygen determination in uranium compounds, in which the sample is attacked by sulfur monochloride. The present paper is concerned with the experimental aspects of the method: apparatus procedure. (authors) [French] Les auteurs ont decrit dans une autre publication (Anal. Chim. Acta) a paraitre, une methode de dosage de l'oxygene dans les composes de l'uranium par attaque par le monochlorure de soufre, La presente note a pour but d'en preciser les techniques experimentale: appareillage, mode operatoire. (auteurs)

  14. Dosage direct des alcools dans les carburols par chromatographie en phase gazeuse Direct Gas Chromatographie Determination of Alcohols in Gasolines Blended by Oxygenated Compounds

    Directory of Open Access Journals (Sweden)

    Petroff N.

    2006-11-01

    Full Text Available Dans cette étude, on décrit une méthode de chromatographie en phase gazeuse utilisant une colonne remplie ; elle permet de doser, sans préfractionnement, les alcools jusqu'aux butanols dans les carburols (carburants additionnés de composés oxygénés. La phase stationnaire sélectionnée est le glycérol. This report describes a gas chromatographie method using a packed column. It allows the direct determination of alcohols up to butanols in gasolines blended with oxygenated compounds without prefractionation. Glycerol has been selected as stationary phase.

  15. Determination of Acid Dissociation Constants (pKa) of Bicyclic Thiohydantoin-Pyrrolidine Compounds in 20% Ethanol-Water Hydroorganic Solvent

    Science.gov (United States)

    Nural, Yahya; Döndaş, H. Ali; Sarı, Hayati; Atabey, Hasan; Belveren, Samet; Gemili, Müge

    2014-01-01

    The acid dissociation constants of potential bioactive fused ring thiohydantoin-pyrrolidine compounds were determined by potentiometric titration in 20% (v/v) ethanol-water mixed at 25 ± 0.1°C, at an ionic background of 0.1 mol/L of NaCl using the HYPERQUAD computer program. Proton affinities of potential donor atoms of the ligands were calculated by AM1 and PM3 semiempiric methods. We found, potentiometrically, three different acid dissociation constants for 1a–f. We suggest that these acid dissociation constants are related to the carboxyl, enol, and amino groups. PMID:24799905

  16. A Simple Analytical Method Using HPLC with Fluorescence Detection to Determine Selected Polycyclic Aromatic Compounds in Filter Samples

    International Nuclear Information System (INIS)

    Garcia, S.; Perez, R. M.

    2014-01-01

    A study on the comparison and evaluation of a miniaturized extraction method for the determination of selected PACs in sample filters is presented. The main objective was the optimization and development of simple, rapid and low cost methods, minimizing the use of extracting solvent volume. The work also includes a study on the intermediate precision. (Author)

  17. Contributions te the study of methods and factors affecting the spectrophotometric determination of boron traces with carmin uranium compounds

    International Nuclear Information System (INIS)

    Fernandez Cellini, R.; Gasco Sanchez, L.

    1956-01-01

    The study of some factors affecting the spectrophotometric determination of boron traces with carmin is made; the influence of carmin from different origin, the stability of complex carmin-boric acid in relation with the sulphuric acid concentration, the interference produced by ion nitrate, and the ion uraline and light influence are discussed. (Author) 36 refs

  18. Approaches to Determining the Oxidation State of Nitrogen and Carbon Atoms in Organic Compounds for High School Students

    Science.gov (United States)

    Jurowski, Kamil; Krzeczkowska, Malgorzata Krystyna; Jurowska, Anna

    2015-01-01

    The concept of oxidation state (or oxidation number) and related issues have always been difficult for students. In addition, there are misunderstandings and obscurities, which can cause improper balancing of the chemical equations (mostly in organic reactions). In particular, these problems are related to determination of the oxidation state of…

  19. Determination of carbon in uranium and its compounds; Determinacion de carbono en uranio metal y sus compuestos

    Energy Technology Data Exchange (ETDEWEB)

    Perez-Garcia, M M

    1972-07-01

    This paper collects the analytical methods used our laboratories for the determination of carbon in uranium metal, uranate salts and the oxides, fluorides and carbides of uranium. The carbon is usually burned off in a induction or resistance oven under oxygen flow. The CO{sub 2} is collected in barite solution. Where it is backtitrated with potassium biphthalate. (Author)

  20. Determination of steroid hormones and related compounds in filtered and unfiltered water by solid-phase extraction, derivatization, and gas chromatography with tandem mass spectrometry

    Science.gov (United States)

    Foreman, William T.; Gray, James L.; ReVello, Rhiannon C.; Lindley, Chris E.; Losche, Scott A.; Barber, Larry B.

    2012-01-01

    A new analytical method has been developed and implemented at the U.S. Geological Survey National Water Quality Laboratory that determines a suite of 20 steroid hormones and related compounds in filtered water (using laboratory schedule 2434) and in unfiltered water (using laboratory schedule 4434). This report documents the procedures and initial performance data for the method and provides guidance on application of the method and considerations of data quality in relation to data interpretation. The analytical method determines 6 natural and 3 synthetic estrogen compounds, 6 natural androgens, 1 natural and 1 synthetic progestin compound, and 2 sterols: cholesterol and 3--coprostanol. These two sterols have limited biological activity but typically are abundant in wastewater effluents and serve as useful tracers. Bisphenol A, an industrial chemical used primarily to produce polycarbonate plastic and epoxy resins and that has been shown to have estrogenic activity, also is determined by the method. A technique referred to as isotope-dilution quantification is used to improve quantitative accuracy by accounting for sample-specific procedural losses in the determined analyte concentration. Briefly, deuterium- or carbon-13-labeled isotope-dilution standards (IDSs), all of which are direct or chemically similar isotopic analogs of the method analytes, are added to all environmental and quality-control and quality-assurance samples before extraction. Method analytes and IDS compounds are isolated from filtered or unfiltered water by solid-phase extraction onto an octadecylsilyl disk, overlain with a graded glass-fiber filter to facilitate extraction of unfiltered sample matrices. The disks are eluted with methanol, and the extract is evaporated to dryness, reconstituted in solvent, passed through a Florisil solid-phase extraction column to remove polar organic interferences, and again evaporated to dryness in a reaction vial. The method compounds are reacted with

  1. Multi-component determination of atmospheric semi-volatile organic compounds in soils and vegetation from Tarragona County, Catalonia, Spain.

    Science.gov (United States)

    Domínguez-Morueco, Noelia; Carvalho, Mariana; Sierra, Jordi; Schuhmacher, Marta; Domingo, José Luis; Ratola, Nuno; Nadal, Martí

    2018-08-01

    Tarragona County (Spain) is home to the most important chemical/petrochemical industrial complex in Southern Europe, which raises concerns about the presence and effects of the numerous environmental contaminants. In order to assess the levels and patterns of five classes of semi-volatile organic compounds (SVOCs) - polycyclic aromatic hydrocarbons (PAHs), synthetic musks (SMs), polychlorinated biphenyls (PCBs), brominated flame retardants (BFRs) and one organochlorine pesticide, hexachlorobenzene (HCB), 27 samples of soil and vegetation (Piptatherum L.) from different areas (petrochemical, chemical, urban/residential, and background) of Tarragona County were analysed. The results show that PAHs levels in soils ranged from 45.12 to 158.00ng/g and the urban areas presented the highest concentrations, mainly associated with the presence of a nearby highway and several roads with heavy traffic. PAHs levels in vegetation samples ranged from 42.13 to 80.08ng/g, where the greatest influence came from the urban and petrochemical areas. In the case of SMs, levels in soils and vegetation samples ranged from 5.42 to 10.04ng/g and from 4.08 to 17.94ng/g, respectively, and in both cases, background areas (at least 30km away from the main SVOCs emission sources) showed the highest levels, suggesting an influence of the personal care products derived from beach-related tourism in the coast. PCBs (from 6.62 to 14.07ng/g in soils; from 0.52 to 4.41ng/g in vegetation) prevailed in the chemical area in both matrices, probably associated with the presence of two sub-electrical stations located in the vicinities. In general terms, BFRs and HCB values recorded in soil and vegetation samples were quite similar between matrices and sampling areas. Copyright © 2018. Published by Elsevier B.V.

  2. In situ and laboratory determined first-order degradation rate constants of specific organic compounds in an aerobic aquifer

    DEFF Research Database (Denmark)

    Nielsen, P.H.; Bjerg, P.L.; Nielsen, P.

    1996-01-01

    In situ microcosms (ISM) and laboratory batch microcosms (LBM) were used for determination of the first-order degradation rate constants of benzene, toluene, o-xylene, nitrobenzene, naphthalene, biphenyl, o- and p-dichlorobenzene, 1,1,1 -trichloroethane, tetrachlorometane, trichloroethene......, tetrachloroethene, phenol, o-cresol, 2,4- and 2,6-dichlorophenol, 4,6-o-dichlorocresol, and o- and p-nitrophenol in an aerobic aquifer, All aromatic hydrocarbons were degraded in ISM and LBM experiments. The phenolic hydrocarbons were ail degraded in ISM experiments, but some failed to degrade in LBM experiments....... Chlorinated aliphatic hydrocarbons were degraded neither in ISM nor LBM experiments. Degradation rate constants were determined by a model accounting for kinetic sorption (bicontinuum model), lag phases, and first-order degradation. With a few exceptions, lag phases were less than 2 weeks in both ISM and LBM...

  3. Calorimetric determination of the heat of precipitation of pseudoephedrine racemic compound--its agreement with the heat of solution.

    Science.gov (United States)

    Pudipeddi, M; Sokoloski, T D; Duddu, S P; Carstensen, J T

    1995-10-01

    The heat of precipitation of dl-pseudoephedrine was determined by direct calorimetry using a Tronac isoperibolic calorimeter. The precipitation of dl-pseudoephedrine was induced by mixing aqueous solutions of the two enantiomers, namely, d- and l-pseudoephedrine, directly in the calorimeter. The molar heat of precipitation of dl-pseudoephedrine was -2.7 and -3.0 kcal/mol at 25 and 30 degrees C, respectively. The aqueous solubility of dl-pseudoephedrine was determined over a temperature range of 20-40 degrees C. The van't Hoff solubility plot was nonlinear. The apparent heat of solution at saturation was obtained from the solubility data using a nonlinear regression model. A good agreement between the magnitude of the apparent heat of solution at saturation and the heat of precipitation was noticed at both 25 and 30 degrees C.

  4. Determination of dissociation constants for coordination compounds of Cr(III) and Co(III) using potentiometric and spectrophotometric methods

    Energy Technology Data Exchange (ETDEWEB)

    Chylewska, A.; Jacewicz, D.; Zarzeczanska, D. [Department of Chemistry, University of Gdansk, Sobieskiego 18/19, 80-952 Gdansk (Poland); Chmurzynski, L. [Department of Chemistry, University of Gdansk, Sobieskiego 18/19, 80-952 Gdansk (Poland)], E-mail: lech@chem.univ.gda.pl

    2008-08-15

    The acid-base properties of analogous complex ions of chromium(III) and cobalt(III) in aqueous solution have been studied. The equilibrium constants for all metal complexes were determined by using potentiometric and spectrophotometric titration methods. First, dissociation constants for the studied complexes of Cr(III) and Co(III) were determined by means of the potentiometric titration method and using the STOICHIO computer programme. Then, pH-spectrophotometric titrations were performed and the OriginPro 7.5 computer programme was used to calculate the same constants. The measurements using both methods were carried out under the same conditions of temperature, T = 298.15 K, and over the same pH range 2.00-10.00, respectively. It turned out that the two methods used enabled us to obtain acidity constants in very good agreement.

  5. Determination of dissociation constants for coordination compounds of Cr(III) and Co(III) using potentiometric and spectrophotometric methods

    International Nuclear Information System (INIS)

    Chylewska, A.; Jacewicz, D.; Zarzeczanska, D.; Chmurzynski, L.

    2008-01-01

    The acid-base properties of analogous complex ions of chromium(III) and cobalt(III) in aqueous solution have been studied. The equilibrium constants for all metal complexes were determined by using potentiometric and spectrophotometric titration methods. First, dissociation constants for the studied complexes of Cr(III) and Co(III) were determined by means of the potentiometric titration method and using the STOICHIO computer programme. Then, pH-spectrophotometric titrations were performed and the OriginPro 7.5 computer programme was used to calculate the same constants. The measurements using both methods were carried out under the same conditions of temperature, T = 298.15 K, and over the same pH range 2.00-10.00, respectively. It turned out that the two methods used enabled us to obtain acidity constants in very good agreement

  6. Determination of Dyclonine Hydrochloride by a HPLC Method and Camphor and Menthol by a GC Method in Compound Lotion

    Directory of Open Access Journals (Sweden)

    Suying Ma

    2013-01-01

    Full Text Available A high performance liquid chromatographic (HPLC method with UV detector for the determination of dyclonine hydrochloride and a gas chromatography (GC method with flame ionization detector (FID for the determination of camphor and menthol in lotion were developed. The developed HPLC method involved using a SinoChoom ODS-BP C18 reversed-phase column (5 μm, 4.6 mm × 200 mm and mobile phase consisting of acetonitrile : water : triethylamine in a ratio of 45 : 55 : 1.0; pH was adjusted to 3.5 with glacial acetic acid. The developed GC method for determination of camphor and menthol involved using an Agilent 19091J-413 capillary chromatographic column (30 m × 320 μm × 0.25 μm. The two methods were validated according to official compendia guidelines. The calibration of dyclonine hydrochloride for HPLC method was linear over the range of 20–200 μg/mL. The retention time was found at 6.0 min for dyclonine hydrochloride. The calibration of camphor and menthol of GC method was linear over the range of 10–2000 μg/mL. The retention time was found at 2.9 min for camphor and 3.05 min for menthol. The proposed HPLC and GC methods were proved to be suitable for the determination of dyclonine hydrochloride, camphor, and menthol in lotion.

  7. Development and validation of an high-performance liquid chromatography-diode array detector method for the simultaneous determination of six phenolic compounds in abnormal savda munziq decoction

    Science.gov (United States)

    Tian, Shuge; Liu, Wenxian; Liu, Feng; Zhang, Xuejia; Upur, Halmuart

    2015-01-01

    Aims: Given the high-effectiveness and low-toxicity of abnormal savda munziq (ASMQ), its herbal formulation has long been used in traditional Uyghur medicine to treat complex diseases, such as cancer, diabetes, and cardiovascular diseases. Settings and Design: ASMQ decoction by reversed-phase high-performance liquid chromatography coupled with a diode array detector was successfully developed for the simultaneous quality assessment of gallic acid, protocatechuic acid, caffeic acid, rutin, rosmarinic acid, and luteolin. The six phenolic compounds were separated on an Agilent TC-C18 reversed-phase analytical column (4.6 × 250 mm, 5 μm) by gradient elution using 0.3% aqueous formic acid (v/v) and 0.3% methanol formic acid (v/v) at 1.0 mL/min. Materials and Methods: The plant material was separately ground and mixed at the following ratios (10): Cordia dichotoma (10.6), Anchusa italic (10.6), Euphorbia humifusa (4.9), Adiantum capillus-veneris (4.9), Ziziphus jujube (4.9), Glycyrrhiza uralensis (7.1), Foeniculum vulgare (4.9), Lavandula angustifolia (4.9), Dracocephalum moldavica L. (4.9), and Alhagi pseudoalhagi (42.3). Statistical Analysis Used: The precisions of all six compounds were Highly significant linear correlations were found between component concentrations and specific chromatographic peak areas (R2 > 0.999). Results: The proposed method was successfully applied to determine the levels of six active components in ASMQ. Conclusions: Given the simplicity, precision, specificity, and sensitivity of the method, it can be utilized as a quality control approach to simultaneously determining the six phenolic compounds in AMSQ. PMID:25709227

  8. X-ray determination of mean square amplitudes of lattice oscillations in compounds with ZnS structure

    International Nuclear Information System (INIS)

    Deus, P.; Schneider, H.A.; Voland, U.

    1980-01-01

    A general method of determination of the mean square amplitudes of lattice oscillations (MSA) for crystals with sphalerite structure is described and applied to InP. The linearity of suitable functions of the measured integral BRAGG intensities of sin 2 theta/lambda 2 is used for the verification of the parameters selected for the correction of extinction and DTS. In this way the accuracy of the results is increased. The MSAs of the InP-sublattices are evaluated. According to theoretical expectations the MSAs of the P-sublattice are larger because of the greater contributions of optical phonons. (author)

  9. Optimization of the Analytical Method Using HPLC with Fluorescence Detection to Determine Selected Polycyclic Aromatic Compounds in Clean Water Samples

    International Nuclear Information System (INIS)

    Garcia Alonso, S.; Perez Pastor, R. M.

    2013-01-01

    A study on the comparison and evaluation of 3 miniaturized extraction methods for the determination of selected PACs in clear waters is presented. Three types of liquid-liquid extraction were used for chromatographic analysis by HPLC with fluorescence detection. The main objective was the optimization and development of simple, rapid and low cost methods, minimizing the use of extracting solvent volume. The work also includes a study on the scope of the methods developed at low and high levels of concentration and intermediate precision. (Author)

  10. Determination of residual volatile organic compounds migrated from polystyrene food packaging into food simulant by headspace solid phase micro extraction-gas chromatography

    International Nuclear Information System (INIS)

    Mohd Marsin Sanagi; Ling, Susie Lu; Zalilah Nasir; Wan Aini Wan Ibrahim; Abu Naim, Ahmedy

    2008-01-01

    The residual styrene and other volatile organic compounds (VOCs) present in the polystyrene food packaging are of concern as these compounds have the potential to migrate into the food in contact. This work describes a method for quantitative determination of VOCs, namely styrene, toluene, ethyl benzene, iso-propylbenzene and n-propylbenzene that have migrated from polystyrene food packaging into food stimulant by gas chromatography-flame ionization detection (GC-FID). Headspace solid phase micro extraction (HS-SPME) technique was applied for migration test using water as food stimulant. The effects of extraction variables including sample volume, eluotropic strength, extraction temperature, extraction time, desorption time, sample agitation, and salt addition on the amounts of the extracted analyses were studied to obtain the optimal HS-SPME conditions. The optimized method was applied to test the VOCs migrated from polystyrene bowls and cups at storage temperatures ranging from 24 to 80 degree Celsius for 30 min. Styrene and ethyl benzene were found to migrate from the samples into the food stimulant. The migration of analyze was found to be strongly dependent upon the storage temperature. The HS-SPME is useful as an alternative method to determine the migration of VOCs from food packaging material into food stimulant. (author)

  11. Antioxidant activity of leaf extracts from different Hibiscus sabdariffa accessions and simultaneous determination five major antioxidant compounds by LC-Q-TOF-MS.

    Science.gov (United States)

    Wang, Jin; Cao, Xianshuang; Jiang, Hao; Qi, Yadong; Chin, Kit L; Yue, Yongde

    2014-12-17

    Hibiscus sabdariffa has gained attention for its antioxidant activity. There are many accessions of H. sabdariffa in the world. However, information on the quantification of antioxidant compounds in different accessions is rather limited. In this paper, a liquid chromatography/quadrupole-time-of-flight mass spectrometry (LC-Q-TOF-MS) method for simultaneous determination of five antioxidant compounds (neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, rutin, and isoquercitrin) in H. sabdariffa leaves was developed. The method was validated for linearity, sensitivity, precision, repeatability and accuracy. The validated method has been successfully applied for determination of the five analytes in eight accessions of H. sabdariffa. The eight accessions of H. sabdariffa were evaluated for their antioxidant activities by DPPH free radical scavenging assay. The investigated accessions of H. sabdariffa were rich in rutin and exhibited strong antioxidant activity. The two accessions showing the highest antioxidant activities were from Cuba (No. 2) and Taiwan (No. 5). The results indicated that H. sabdariffa leaves could be considered as a potential antioxidant source for the food industry. The developed LC-Q-TOF-MS method is helpful for quality control of H. sabdariffa.

  12. A gravimetric method for the determination of oxygen in uranium oxides and ternary uranium oxides by addition of alkaline earth compounds

    International Nuclear Information System (INIS)

    Fujino, Takeo; Tagawa, Hiroaki; Adachi, Takeo; Hashitani, Hiroshi

    1978-01-01

    A simple gravimetric determination of oxygen in uranium oxides and ternary uranium oxides is described. In alkaline earth uranates which are formed by heating in air at 800-1100 0 C, uranium is in the hexavalent state over certain continuous ranges of alkaline earth-to-uranium ratios. Thus, if an alkaline earth uranate or a compound containing an alkaline earth element, e.g. MgO, is mixed with the oxide sample and heated in air under suitable conditions, oxygen can be determined from the weight change before and after the reaction. The standard deviation of the O:U ratio for a UOsub(2+x) test sample is +-0.0008-0.001, if a correction is applied for atmospheric moisture absorbed during mixing. (Auth.)

  13. Synthesis by two methods and crystal structure determination of a new pyrochlore-related compound Sm{sub 2}FeTaO{sub 7}

    Energy Technology Data Exchange (ETDEWEB)

    Torres-Martinez, Leticia M., E-mail: lettorresg@yahoo.com [Departamento de Ecomateriales y Energia, Facultad de Ingenieria Civil, Universidad Autonoma de Nuevo Leon, Cd. Universitaria, San Nicolas de los Garza, Nuevo Leon 66450 (Mexico); Ruiz-Gomez, Miguel A. [Departamento de Ecomateriales y Energia, Facultad de Ingenieria Civil, Universidad Autonoma de Nuevo Leon, Cd. Universitaria, San Nicolas de los Garza, Nuevo Leon 66450 (Mexico); Facultad de Ciencias Quimicas, Universidad Autonoma de San Luis Potosi, Av. Manuel Nava 6, San Luis Potosi, S.L.P. 78290 (Mexico); Figueroa-Torres, M.Z.; Juarez-Ramirez, Isaias [Departamento de Ecomateriales y Energia, Facultad de Ingenieria Civil, Universidad Autonoma de Nuevo Leon, Cd. Universitaria, San Nicolas de los Garza, Nuevo Leon 66450 (Mexico); Moctezuma, Edgar [Facultad de Ciencias Quimicas, Universidad Autonoma de San Luis Potosi, Av. Manuel Nava 6, San Luis Potosi, S.L.P. 78290 (Mexico); and others

    2012-04-16

    Graphical abstract: The monoclinic (space group C2/c) structure of a new compound, Sm{sub 2}FeTaO{sub 7} shows an alternating Sm-O and Fe/Ta-O layers. In the Fe/Ta-O layer, Fe/Ta1 and Fe/Ta3 cations are coordinated by six oxygen atoms, forming irregular octahedral interconnected into a hexagonal tungsten bronze (HTB) type network. The HTB layer is a fundamental framework in the pyrohlore-related structure. Highlights: Black-Right-Pointing-Pointer Pyrochlore-related compound Sm{sub 2}FeTaO{sub 7} prepared by solid state reaction and sol-gel. Black-Right-Pointing-Pointer Sm{sub 2}FeTaO{sub 7} crystallizes with a monoclinic crystal structure and space group C2/c. Black-Right-Pointing-Pointer The compound is synthesized by sol-gel at lower temperature and time than solid state. Black-Right-Pointing-Pointer Surface area of sol-gel Sm{sub 2}FeTaO{sub 7} is 10 times higher than that prepared by solid state. - Abstract: This paper reports on the synthesis of a new pyrochlore-related compound Sm{sub 2}FeTaO{sub 7} by both solid state reaction and sol-gel synthesis routes. Structural features were determined by X-ray powder diffraction and Rietveld refinement and were corroborated using Transmission Electron Microscopy (TEM). The results revealed that Sm{sub 2}FeTaO{sub 7} crystallized in the monoclinic system with space group C2/c and the following cell parameters: a = 13.1307(5) Angstrom-Sign , b = 7.5854(3) Angstrom-Sign , c = 11.6425(4) Angstrom-Sign and {beta} = 100.971(2) Degree-Sign . The monoclinic structure of Sm{sub 2}FeTaO{sub 7} showed an arrangement of alternating Sm-O and Fe/Ta-O layers and two types of irregular octahedra of Fe/Ta-O, which are interconnected into a hexagonal tungsten bronze (HTB)-type network. On the other hand, Sm{sub 2}FeTaO{sub 7} prepared by sol-gel was obtained with lower particle sizes than the solid state produced compound. The difference in particle size causes a difference of one order of magnitude in the specific surface area. In

  14. Biogenic volatile organic compound (BVOC) emissions from forested areas in Turkey: determination of specific emission rates for thirty-one tree species.

    Science.gov (United States)

    Aydin, Yagmur Meltem; Yaman, Baris; Koca, Husnu; Dasdemir, Okan; Kara, Melik; Altiok, Hasan; Dumanoglu, Yetkin; Bayram, Abdurrahman; Tolunay, Doganay; Odabasi, Mustafa; Elbir, Tolga

    2014-08-15

    Normalized biogenic volatile organic compound (BVOC) emission rates for thirty one tree species that cover the 98% of national forested areas in Turkey were determined. Field samplings were performed at fourteen different forested areas in Turkey using a specific dynamic enclosure system. The selected branches of tree species were enclosed in a chamber consisted of a transparent Nalofan bag. The air-flows were sampled from both inlet and outlet of the chamber by Tenax-filled sorbent tubes during photosynthesis of trees under the presence of sunlight. Several environmental parameters (temperature, humidity, photosynthetically active radiation-PAR, and CO2) were continuously monitored inside and outside the enclosure chamber during the samplings. Collected samples were analyzed using a gas chromatography mass spectrometry (GC/MS) system equipped with a thermal desorber (TD). Sixty five BVOCs classified in five major groups (isoprene, monoterpenes, sesquiterpenes, oxygenated sesquiterpenes, and other oxygenated compounds) were analyzed. Emission rates were determined by normalization to standard conditions (1000 μmol/m(2)s PAR and 30 °C temperature for isoprene and 30 °C temperature for the remaining compounds). In agreement with the literature, isoprene was mostly emitted by broad-leaved trees while coniferous species mainly emitted monoterpenes. Several tree species such as Sweet Chestnut, Silver Lime, and European Alder had higher monoterpene emissions although they are broad-leaved species. High isoprene emissions were also observed for a few coniferous species such as Nordmann Fir and Oriental Spruce. The highest normalized total BVOC emission rate of 27.1 μg/gh was observed for Oriental Plane while South European Flowering Ash was the weakest BVOC emitter with a total normalized emission rate of 0.031 μg/gh. Monoterpene emissions of broad-leaved species mainly consisted of sabinene, limonene and trans-beta-ocimene, while alpha-pinene, beta-pinene and beta

  15. Application of high performance liquid chromatography with inductively coupled plasma mass spectrometry (HPLC-ICP-MS) for determination of chromium compounds in the air at the workplace.

    Science.gov (United States)

    Stanislawska, Magdalena; Janasik, Beata; Wasowicz, Wojciech

    2013-12-15

    The toxicity and bioavailability of chromium species are highly dependable on the form or species, therefore determination of total chromium is insufficient for a complete toxicological evaluation and risk assessment. An analytical method for determination of soluble and insoluble Cr (III) and Cr (VI) compounds in welding fume at workplace air has been developed. The total chromium (Cr) was determined by using quadruple inductively coupled plasma mass spectrometry (ICP-MS) equipped with a dynamic reaction cell (DRC(®)). Soluble trivalent and hexavalent chromium compounds were determined by high performance liquid chromatography with inductively coupled plasma mass spectrometry (HPLC-ICP-MS). A high-speed, reversed-phase CR C8 column (PerkinElmer, Inc., Shelton, CT, USA) was used for the speciation of soluble Cr (III) and soluble Cr (VI). The separation was accomplished by interaction of the chromium species with the different components of the mobile phase. Cr (III) formed a complex with EDTA, i.e. retained on the column, while Cr (VI) existed in the solutions as dichromate. Alkaline extraction (2% KOH and 3% Na2CO3) and anion exchange column (PRP-X100, PEEK, Hamilton) were used for the separation of the total Cr (VI). The results of the determination of Cr (VI) were confirmed by the analysis of the certified reference material BCR CRM 545 (Cr (VI) in welding dust). The results obtained for the certified material (40.2±0.6 g kg(-1)) and the values recorded in the examined samples (40.7±0.6 g kg(-1)) were highly consistent. This analytical method was applied for the determination of chromium in the samples in the workplace air collected onto glass (Whatman, Ø 37 mm) and membrane filters (Sartorius, 0.8 μm, Ø 37 mm). High performance liquid chromatography with inductively coupled plasma mass spectrometry is a remarkably powerful and versatile technique for determination of chromium species in welding fume at workplace air. Crown Copyright © 2013 Published by

  16. Determination of mustard and lewisite related compounds in abandoned chemical weapons (Yellow shells) from sources in China and Japan.

    Science.gov (United States)

    Hanaoka, Shigeyuki; Nomura, Koji; Wada, Takeharu

    2006-01-06

    Knowledge of the states of the contents in chemical munitions that Japanese Imperial Forces abandoned at the end of World War II in Japan and China is gravely lacking. To unearth and recover these chemical weapons and detoxify the contents safely, it is essential to establish analytical procedures to definitely determine the CWA contents. We established such a procedure and applied it to the analysis of chemicals in the abandoned shells. Yellow shells are known to contain sulfur mustard, lewisite, or a mixture of both. Lewisite was analyzed without thiol derivatization, because it and its decomposition products yield the same substances in the derivatization. Analysis using our new procedure showed that both mustard and lewisite remained as the major components after the long abandonment of nearly 60 years. The content of mustard was 43% and that of lewisite 55%. The viscous material found was suggested to be mostly oligomers of mustard. Comparison of the components in the Yellow agents with mustard recovered in both Japan and China showed a difference in the impurities between the CWAs produced by the former Imperial navy and those by the former Imperial army.

  17. Workers make the queens in melipona bees: identification of geraniol as a caste determining compound from labial glands of nurse bees.

    Science.gov (United States)

    Jarau, Stefan; van Veen, Johan W; Twele, Robert; Reichle, Christian; Gonzales, Eduardo Herrera; Aguilar, Ingrid; Francke, Wittko; Ayasse, Manfred

    2010-06-01

    Reproductive division of labor in advanced eusocial honey bees and stingless bees is based on the ability of totipotent female larvae to develop into either workers or queens. In nearly all species, caste is determined by larval nutrition. However, the mechanism that triggers queen development in Melipona bees is still unresolved. Several hypotheses have been proposed, ranging from the proximate (a genetic determination of caste development) to the ultimate (a model in which larvae have complete control over their own caste fate). Here, we showed that the addition of geraniol, the main compound in labial gland secretions of nurse workers, to the larval food significantly increases the number of larvae that develop into queens. Interestingly, the proportion of queens in treated brood exactly matched the value (25%) predicted by the two-locus, two-allele model of genetic queen determination, in which only females that are heterozygous at both loci are capable of developing into queens. We conclude that labial gland secretions, added to the food of some cells by nurse bees, trigger queen development, provided that the larvae are genetically predisposed towards this developmental pathway. In Melipona beecheii, geraniol acts as a primer pheromone representing the first caste determination substance identified to date.

  18. Band structures of 4f and 5f materials studied by angle-resolved photoelectron spectroscopy.

    Science.gov (United States)

    Fujimori, Shin-ichi

    2016-04-20

    Recent remarkable progress in angle-resolved photoelectron spectroscopy (ARPES) has enabled the direct observation of the band structures of 4f and 5f materials. In particular, ARPES with various light sources such as lasers (hν ~ 7 eV) or high-energy synchrotron radiations (hν >/~ 400 eV) has shed light on the bulk band structures of strongly correlated materials with energy scales of a few millielectronvolts to several electronvolts. The purpose of this paper is to summarize the behaviors of 4f and 5f band structures of various rare-earth and actinide materials observed by modern ARPES techniques, and understand how they can be described using various theoretical frameworks. For 4f-electron materials, ARPES studies of CeMIn5(M = Rh, Ir, and Co) and YbRh2Si2 with various incident photon energies are summarized. We demonstrate that their 4f electronic structures are essentially described within the framework of the periodic Anderson model, and that the band-structure calculation based on the local density approximation cannot explain their low-energy electronic structures. Meanwhile, electronic structures of 5f materials exhibit wide varieties ranging from itinerant to localized states. For itinerant U5f compounds such as UFeGa5, their electronic structures can be well-described by the band-structure calculation assuming that all U5f electrons are itinerant. In contrast, the band structures of localized U5f compounds such as UPd3 and UO2 are essentially explained by the localized model that treats U5f electrons as localized core states. In regards to heavy fermion U-based compounds such as the hidden-order compound URu2Si2, their electronic structures exhibit complex behaviors. Their overall band structures are generally well-explained by the band-structure calculation, whereas the states in the vicinity of EF show some deviations due to electron correlation effects. Furthermore, the electronic structures of URu2Si2 in the paramagnetic and hidden-order phases are

  19. IN VITRO INHIBITION OF CELERY (Apium graveolens L. EXTRACT ON THE ACTIVITY OF XANTHINE OXIDASE AND DETERMINATION OF ITS ACTIVE COMPOUND

    Directory of Open Access Journals (Sweden)

    Dyah Iswantini

    2012-12-01

    Full Text Available The objective of this study was to determine the inhibition effect of celery extracts toward xanthine oxidase by in vitro method, and its active compounds. Roots and herb of celery were extracted using water and ethanol solvents. Results indicated that the herbal ethanol extract had the highest inhibition effect (91.40% at 1400 ppm. The components contained in the herbal ethanol extract were then separated by column chromatography using the best eluent (chloroform : ethyl acetate at 7:3. All of the fractions had inhibition effect greater than 50%. The fraction number 4 was the one with the highest inhibition effect followed by fraction 5 with inhibition percentage of both fractions at 200 ppm were 88.62 and 85.44%, respectively. The analysis of the ultraviolet spectrum of fraction 4 showed the presence of π-π* transition which was resulted by the aromatic C=C, -OH, and C-O chromophores, and also showing the n-σ* transition which was given by -C=O chromophore. The infrared spectrum analysis indicated the presence of aromatic -C=C, -OH, and C=O functional groups. Based on the phytochemical assay and both instrumental spectrums, it was thought that the active compounds of fraction 4 and 5 were in the flavonoid group.

  20. Ab initio structure determination of nanocrystals of organic pharmaceutical compounds by electron diffraction at room temperature using a Timepix quantum area direct electron detector

    Energy Technology Data Exchange (ETDEWEB)

    Genderen, E. van; Clabbers, M. T. B. [Biophysical Structural Chemistry, Leiden University, Einsteinweg 55, 2333 CC Leiden (Netherlands); Center for Cellular Imaging and NanoAnalytics (C-CINA), Biozentrum, University of Basel, CH-4058 Basel (Switzerland); Das, P. P. [Nanomegas SPRL, Boulevard Edmond Machtens 79, B 1080, Brussels (Belgium); Stewart, A. [Department of Physics and Energy, Materials and Surface Science Institute (MSSI), University of Limerick, Limerick (Ireland); Nederlof, I. [Biophysical Structural Chemistry, Leiden University, Einsteinweg 55, 2333 CC Leiden (Netherlands); Amsterdam Scientific Instruments, Postbus 41882, 1009 DB Amsterdam (Netherlands); Barentsen, K. C. [Biophysical Structural Chemistry, Leiden University, Einsteinweg 55, 2333 CC Leiden (Netherlands); Portillo, Q. [Nanomegas SPRL, Boulevard Edmond Machtens 79, B 1080, Brussels (Belgium); Centres Científics i Tecnològics de la Universitat de Barcelona, University of Barcelona, Carrer de Lluís Solé i Sabaris, 1-3, Barcelona (Spain); Pannu, N. S. [Biophysical Structural Chemistry, Leiden University, Einsteinweg 55, 2333 CC Leiden (Netherlands); Nicolopoulos, S. [Nanomegas SPRL, Boulevard Edmond Machtens 79, B 1080, Brussels (Belgium); Gruene, T., E-mail: tim.gruene@psi.ch [Biology and Chemistry, Laboratory of Biomolecular Research, Paul Scherrer Institute (PSI), 5232 Villigen (Switzerland); Abrahams, J. P., E-mail: tim.gruene@psi.ch [Biophysical Structural Chemistry, Leiden University, Einsteinweg 55, 2333 CC Leiden (Netherlands); Center for Cellular Imaging and NanoAnalytics (C-CINA), Biozentrum, University of Basel, CH-4058 Basel (Switzerland); Biology and Chemistry, Laboratory of Biomolecular Research, Paul Scherrer Institute (PSI), 5232 Villigen (Switzerland)

    2016-02-05

    A specialized quantum area detector for electron diffraction studies makes it possible to solve the structure of small organic compound nanocrystals in non-cryo conditions by direct methods. Until recently, structure determination by transmission electron microscopy of beam-sensitive three-dimensional nanocrystals required electron diffraction tomography data collection at liquid-nitrogen temperature, in order to reduce radiation damage. Here it is shown that the novel Timepix detector combines a high dynamic range with a very high signal-to-noise ratio and single-electron sensitivity, enabling ab initio phasing of beam-sensitive organic compounds. Low-dose electron diffraction data (∼0.013 e{sup −} Å{sup −2} s{sup −1}) were collected at room temperature with the rotation method. It was ascertained that the data were of sufficient quality for structure solution using direct methods using software developed for X-ray crystallography (XDS, SHELX) and for electron crystallography (ADT3D/PETS, SIR2014)

  1. Direct determination of N-methyl-2-pyrrolidone metabolites in urine by HPLC-electrospray ionization-MS/MS using deuterium-labeled compounds as internal standard.

    Science.gov (United States)

    Suzuki, Yoshihiro; Endo, Yoko; Ogawa, Masanori; Yamamoto, Shinobu; Takeuchi, Akito; Nakagawa, Tomoo; Onda, Nobuhiko

    2009-11-01

    N-methyl-2-pyrrolidone (NMP) has been used in many industries and biological monitoring of NMP exposure is preferred to atmospheric monitoring in occupational health. We developed an analytical method that did not include solid phase extraction (SPE) but utilized deuterium-labeled compounds as internal standard for high-performance liquid chromatography-electrospray ionization-mass spectrometry using a C30 column. Urinary concentrations of NMP and its known metabolites 5-hydoxy-N-methyl-2-pyrrolidone (5-HNMP), N-methyl-succinimide (MSI), and 2-hydroxy-N-methylsuccinimide (2-HMSI) were determined in a single run. The method provided baseline separation of these compounds. Their limits of detection in 10-fold diluted urine were 0.0001, 0.006, 0.008, and 0.03 mg/L, respectively. Linear calibration covered a biological exposure index (BEI) for urinary concentration. The within-run and total precisions (CV, %) were 5.6% and 9.2% for NMP, 3.4% and 4.2% for 5-HNMP, 3.7% and 6.0% for MSI, and 6.5% and 6.9% for 2-HMSI. The method was evaluated using international external quality assessment samples, and urine samples from workers exposed to NMP in an occupational area.

  2. Quantification of prominent volatile compounds responsible for muskmelon and watermelon aroma by purge and trap extraction followed by gas chromatography-mass spectrometry determination.

    Science.gov (United States)

    Fredes, Alejandro; Sales, Carlos; Barreda, Mercedes; Valcárcel, Mercedes; Roselló, Salvador; Beltrán, Joaquim

    2016-01-01

    A dynamic headspace purge-and-trap (DHS-P&T) methodology for the determination and quantification of 61 volatile compounds responsible for muskmelon and watermelon aroma has been developed and validated. The methodology is based on the application of purge-and-trap extraction followed by gas chromatography coupled to (ion trap) mass spectrometry detection. For this purpose two different P&T sorbent cartridges have been evaluated. The influence of different extraction factors (sample weight, extraction time, and purge flow) on extraction efficiency has been studied and optimised using response surface methodology. Precision, expressed as repeatability, has been evaluated by analysing six replicates of real samples, showing relative standard deviations between 3% and 27%. Linearity has been studied in the range of 10-6130 ng mL(-1) depending on the compound response, showing coefficients of correlation between 0.995 and 0.999. Detection limits ranged between 0.1 and 274 ng g(-1). The methodology developed is well suited for analysis of large numbers of muskmelon and watermelon samples in plant breeding programs. Copyright © 2015 Elsevier Ltd. All rights reserved.

  3. Sediment Origin Determination in the Sub-Catchment of Mistelbach (Austria) using Fatty Acids Biomarkers and Compound-Specific Stable Isotope Techniques

    International Nuclear Information System (INIS)

    Mabit, L.; Chen, X.; Resch, C.; Toloza, A.; Meusburger, K.; Alewell, C.; Gibbs, M.; Klik, A.; Eder, A.; Strauss, P.

    2016-01-01

    Compound-specific stable isotope (CSSI) signatures of inherent soil organic biomarkers allow discriminating and apportioning the source of soil contribution from different land uses. Plant communities label the soil where they grow by exuding organic biomarkers. Although all plants produce the same biomarkers, the stable isotopic signature of those biomarkers is different for each plant species. For agri-environmental investigations, the CSSI technique is based on the measurement of carbon-13 ( 13 C) natural abundance signatures of specific organic compounds such as natural fatty acids (FAs) in the soil. By linking fingerprints of land use to the sediment in deposition zones, this approach has been shown to be a useful technique for determining the source of eroded soil and thereby identifying areas prone to soil degradation. The authors have used this innovative technique to investigate a 3 hectares sub-catchment of Mistelbach situated 60 km north of Vienna. Using the 137 Cs technique, Mabit et al. (2009) reported a local maximum sedimentation rate reaching 20 to 50 t ha -1 yr -1 in the lowest part of this Austrian catchment. To test the ability of the CSSI technique to discriminate different sediment sources of these deposited sediments, representative soil samples from four main agricultural fields of the site were analyzed

  4. High-performance liquid chromatography using reversed-phase stationary phases dynamically modified with organophosphorus compound for the separation and determination of lanthanoid elements

    International Nuclear Information System (INIS)

    Tsuyoshi, Akira; Akiba, Kenichi

    2000-01-01

    An acidic organophosphorus compound, 2-ethylhexylphosphonic acid mono-2-ethlhexyl ester (EHPA), has been applied to reversed-phase high-performance liquid chromatography (RP-HPLC). The reversed-phase stationary phase was dynamically modified with EHPA by flowing the mobile phase of an acetone-water mixture containing the extracting regent. The retention of lanthanoid elements was widely varied by changing the conditions of the mobile phase, i.e., the pH, the EHPA concentration and the acetone content. The selectivity of EHPA is well reflected to the chromatographic systems, and a precise separation of lanthanoid elements was achieved with sufficient resolution. The determination of Sm was examined in the presence of a large amount of Nd. A linear calibration graph was obtained for Sm at the level of 10 -7 mol dm -3 , in the presence of 1x10 -4 mol dm -3 of Nd. (author)

  5. Solid-phase microextraction method for the determination of hexanal in hazelnuts as an indicator of the interaction of active packaging materials with food aroma compounds.

    Science.gov (United States)

    Pastorelli, S; Valzacchi, S; Rodriguez, A; Simoneau, C

    2006-11-01

    Fatty foods are susceptible to lipid oxidation resulting in deterioration of product quality due to the generation of off-flavours. Hexanal is a good indicator of rancidity. Therefore, a method based on solid-phase microextraction (SPME) coupled to gas chromatograph with flame ionization detection was developed to determine hexanal formation in hazelnuts during storage. Optimum conditions were as follows: carboxen-polydimethylsiloxane 75 microm fibre, extraction time 10 min, equilibrium time 10 min and equilibrium temperature 60 degrees C. The effect of oxygen scavengers on the oxidation process was also evaluated by measuring hexanal formation in hazelnuts stored with/without oxygen absorber sachets. Oxygen scavengers were shown to reduce oxidation; however, analysis of the sachet revealed that other volatile compounds from the headspace were also absorbed.

  6. Organosulphur Compounds in Coals as Determined by Reaction with Raney Nickel and Microscale Pyrolysis Techniques. Quarterly report, January-March, 1996

    International Nuclear Information System (INIS)

    Stalker, L.; Philip, P.

    1997-01-01

    Since the last report, we have concentrated on completing all the chemical degradation experimental work. This has involved the completion of a series of chemical degradation experiments using deuterium labeled sodium borohydride and deuterated methanol . The products of these desulphurization experiments have, as usual, been fractionated into aliphatic and aromatic hydrocarbons and NSO compounds. The aliphatic hydrocarbon fractions of each desulphurization experiment are currently being analysed by gas chromatography(GC) and gas chromatography-mass spectrometry(GCMS). The object of the deuterium labelling experiments is to determine the relative abundance of thioether, triolane, and thiophene organic sulphur units cleaved in the different coal fractions( i.e. pre- extracted coal matrix, asphaltene and free polars from the maltenes)

  7. The Use of Silver Solid Amalgam Electrodes for Voltammetric and Amperometric Determination of Nitrated Polyaromatic Compounds Used as Markers of Incomplete Combustion

    Directory of Open Access Journals (Sweden)

    Oksana Yosypchuk

    2012-01-01

    Full Text Available Genotoxic nitrated polycyclic aromatic hydrocarbons (NPAHs are formed during incomplete combustion processes by reaction of polycyclic aromatic hydrocarbons (PAHs with atmospheric nitrogen oxides. 1-Nitropyrene, 2-nitrofluorene, and 3-nitrofluoranthene as the dominating substances are used as markers of NPAHs formation by these processes. In the presented study, voltammetric properties and quantification of these compounds and of 5-nitroquinoline (as a representative of environmentally important genotoxic heterocyclic compounds have been investigated using a mercury meniscus modified silver solid amalgam electrode (m-AgSAE, which represent a nontoxic alternative to traditional mercury electrodes. Linear calibration curves over three orders of magnitude and limits of determination mostly in the 10−7 mol L−1 concentration range were obtained using direct current and differential pulse voltammetry. Further, satisfactory HPLC separation of studied analytes in fifteen minutes was achieved using 0.01 mol L−1 phosphate buffer, pH 7.0 : methanol (15 : 85, v/v mobile phase, and C18 reversed stationary phase. Limits of detection of around 1 · 10−5 mol L−1 were achieved using amperometric detection at m-AgSAE in wall-jet arrangement for all studied analytes. Practical applicability of this technique was demonstrated on the determination of 1-nitropyrene, 2-nitrofluorene, 3-nitrofluoranthene, and 5-nitroquinoline in drinking water after their preliminary separation and preconcentration using solid phase extraction with the limits of detection around 1 · 10−6 mol L−1.

  8. Determination of quaternary ammonium compounds in oranges and cucumbers using QuEChERS extraction and ultra-performance liquid chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Arrebola-Liébanas, Francisco Javier; Abdo, María Angeles Herrera; Moreno, José Luis Fernandez; Martínez-Vidal, José L; Frenich, Antonia Garrido

    2014-01-01

    A simple and fast method has been developed for determining relevant quaternary ammonium compounds in cucumber and orange samples. The target compounds were benzoalkonium chloride (BAC-10, BAC-12, BAC-14, and BAC-16), didecyldimethylammonium chloride, and benzethonium chloride, all frequently used biocides in the agrifood industry. An extraction based on the buffered Quick, Easy, Cheap, Effective, Rugged, and Safe method and determination by ultra-performance LC/MS/MS that eluted the biocides in less than 5 min were used. The method was fully validated and implemented in a UNE-EN-ISO/IEC 17025 accredited laboratory for its application to the analysis of real samples. Performance characteristics of the method are reported, including an estimation of measurement uncertainty. Calibration curves were set between 0.01 and 0.150 mg/kg, LOD values were always between 0.4 and 1.0 microg/kg, LOQ values were in the range 1-4 microg/kg, recovery was between 81 and 115%, intraday and interday precision were always lower than 17% (expressed as RSD), and expanded uncertainty was always lower than 40%. The validation was accomplished for the two studied matrixes at spiking concentrations of 0.011 and 0.050 mg/kg. The method has been applied to the analysis of 30 cucumber and orange samples that were found to contain concentrations of BAC-12 that ranged between 0.015 and 0.210 mg/kg and of BAC-14 between 0.018 and 0.081 mg/kg.

  9. Acid dissociation constants of uridine-5 Prime -diphosphate compounds determined by {sup 31}phosphorus nuclear magnetic resonance spectroscopy and internal pH referencing

    Energy Technology Data Exchange (ETDEWEB)

    Jancan, Igor [Louisiana State University, Department of Chemistry, Baton Rouge, LA 70803 (United States); Macnaughtan, Megan A., E-mail: macnau@lsu.edu [Louisiana State University, Department of Chemistry, Baton Rouge, LA 70803 (United States)

    2012-10-24

    Highlights: Black-Right-Pointing-Pointer The first reported phosphate and imide pK{sub a} values of UDP-GlcNAc and UDP-S-GlcNAc. Black-Right-Pointing-Pointer New role for the monosaccharide in the imide pK{sub a} of uridine-5 Prime -phosphate compounds. Black-Right-Pointing-Pointer UDP-S-GlcNAc and UDP-GlcNAc have the same phosphate pK{sub a}, unlike thioyl analogs. Black-Right-Pointing-Pointer The {sup 31}P chemical shift of inorganic phosphate is a viable internal pH reference. Black-Right-Pointing-Pointer Stability of the external {sup 31}P chemical shift reference is essential. - Abstract: The acid dissociation constant (pK{sub a}) of small, biological molecules is an important physical property used for investigating enzyme mechanisms and inhibitor design. For phosphorus-containing molecules, the {sup 31}P nuclear magnetic resonance (NMR) chemical shift is sensitive to the local chemical environment, particularly to changes in the electronic state of the molecule. Taking advantage of this property, we present a {sup 31}P NMR approach that uses inorganic phosphate buffer as an internal pH reference to determine the pK{sub a} values of the imide and second diphosphate of uridine-5 Prime -diphosphate compounds, including the first reported values for UDP-GlcNAc and UDP-S-GlcNAc. New methods for using inorganic phosphate buffer as an internal pH reference, involving mathematical correction factors and careful control of the chemical shift reference sample, are illustrated. A comparison of the newly determined imide and diphosphate pK{sub a} values of UDP, UDP-GlcNAc, and UDP-S-GlcNAc with other nucleotide phosphate and thio-analogs reveals the significance of the monosaccharide and sulfur position on the pK{sub a} values.

  10. Single-laboratory validation of a method for the determination of select volatile organic compounds in foods by using vacuum distillation with gas chromatography/mass spectrometry.

    Science.gov (United States)

    Nyman, Patricia J; Limm, William; Begley, Timothy H; Chirtel, Stuart J

    2014-01-01

    Recent studies showed that headspace and purge and trap methods have limitations when used to determine volatile organic compounds (VOCs) in foods, including matrix effects and artifact formation from precursors present in the sample matrix or from thermal decomposition. U.S. Environmental Protection Agency Method 8261A liberates VOCs from the sample matrix by using vacuum distillation at room temperature. The method was modified and validated for the determination of furan, chloroform, benzene, trichloroethene, toluene, and sytrene in infant formula, canned tuna (in water), peanut butter, and an orange beverage (orange-flavored noncarbonated beverage). The validation studies showed that the LOQ values ranged from 0.05 ng/g toluene in infant formula to 5.10 ng/g toluene in peanut butter. Fortified recoveries were determined at the first, second, and third standard additions, and concentrations ranged from 0.07 to 6.9 ng/g. When quantified by the method of standard additions, the recoveries ranged from 56 to 218% at the first standard addition and 89 to 117% at the third. The validated method was used to conduct a survey of the targeted VOCs in 18 foods. The amounts found ranged from none detected to 73.8 ng/g furan in sweet potato baby food.

  11. Biogenic volatile organic compounds (BVOCs) emission of Scots pine under drought stress - a 13CO2 labeling study to determine de novo and pool emissions under different treatments

    Science.gov (United States)

    Lüpke, M.

    2015-12-01

    Plants emit biogenic volatile organic compounds (BVOCs) to e.g. communicate and to defend herbivores. Yet BVOCs also impact atmospheric chemistry processes, and lead to e.g. the built up of secondary organic aerosols. Abiotic stresses, such as drought, however highly influence plant physiology and subsequently BVOCs emission rates. In this study, we investigated the effect of drought stress on BVOCs emission rates of Scots pine trees, a de novo and pool emitter, under controlled climate chamber conditions within a dynamic enclosure system consisting of four plant chambers. Isotopic labeling with 13CO2 was used to detect which ratio of emissions of BVOCs derives from actual synthesis and from storage organs under different treatments. Additionally, the synthesis rate of the BVOCs synthesis can be determined. The experiment consisted of two campaigns (July 2015 and August 2015) of two control and two treated trees respectively in four controlled dynamic chambers simultaneously. Each campaign lasted for around 21 days and can be split into five phases: adaptation, control, dry-out, drought- and re-watering phase. The actual drought phase lasted around five days. During the campaigns two samples of BVOCs emissions were sampled per day and night on thermal desorption tubes and analyzed by a gas chromatograph coupled with a mass spectrometer and a flame ionization detector. Additionally, gas exchange of water and CO2, soil moisture, as well as leaf and chamber temperature was monitored continuously. 13CO2 labeling was performed simultaneously in all chambers during the phases control, drought and re-watering for five hours respectively. During the 13CO2 labeling four BVOCs emission samples per chamber were taken to identify the labeling rate on emitted BVOCs. First results show a decrease of BVOCs emissions during the drought phase and a recovery of emission after re-watering, as well as different strength of reduction of single compounds. The degree of labeling with 13

  12. Quantitative determination of biological activity of botulinum toxins utilizing compound muscle action potentials (CMAP), and comparison of neuromuscular transmission blockage and muscle flaccidity among toxins.

    Science.gov (United States)

    Torii, Yasushi; Goto, Yoshitaka; Takahashi, Motohide; Ishida, Setsuji; Harakawa, Tetsuhiro; Sakamoto, Takashi; Kaji, Ryuji; Kozaki, Shunji; Ginnaga, Akihiro

    2010-01-01

    The biological activity of various types of botulinum toxin has been evaluated using the mouse intraperitoneal LD(50) test (ip LD(50)). This method requires a large number of mice to precisely determine toxin activity, and so has posed a problem with regard to animal welfare. We have used a direct measure of neuromuscular transmission, the compound muscle action potential (CMAP), to evaluate the effect of different types of botulinum neurotoxin (NTX), and we compared the effects of these toxins to evaluate muscle relaxation by employing the digit abduction scoring (DAS) assay. This method can be used to measure a broad range of toxin activities the day after administration. Types A, C, C/D, and E NTX reduced the CMAP amplitude one day after administration at below 1 ip LD(50), an effect that cannot be detected using the mouse ip LD(50) assay. The method is useful not only for measuring toxin activity, but also for evaluating the characteristics of different types of NTX. The rat CMAP test is straightforward, highly reproducible, and can directly determine the efficacy of toxin preparations through their inhibition of neuromuscular transmission. Thus, this method may be suitable for pharmacology studies and the quality control of toxin preparations. Copyright 2009 Elsevier Ltd. All rights reserved.

  13. Optimization of an analytical methodology for the determination of alkyl- and methoxy-phenolic compounds by HS-SPME in biomass smoke

    Energy Technology Data Exchange (ETDEWEB)

    Conde, Francisco J.; Afonso, Ana M.; Gonzalez, Venerando; Ayala, Juan H. [University of La Laguna, Campus de Anchieta, Department of Analytical Chemistry, Nutrition and Food Science, La Laguna (Spain)

    2006-08-15

    A sampling and analysis method for the determination of 21 phenolic compounds in smoke samples from biomass combustion has been developed. The smoke is used to make smoked foods, following an artisanal procedure used in some parts of the Canary Islands. The sampling system consists of a Bravo H air sampler, two impingers, each one containing an aqueous solution of sodium hydroxide 0.1 mol L{sup -1}, followed by a silica gel trap. The variables optimized to reach the best sampling conditions were volume of absorbent solution and sampling flow. Under the optimum conditions, 100 mL of absorbent solution of NaOH 0.10 mol L{sup -1} and 2 L min{sup -1} for the sampling flow, sampling efficiencies are higher than 80%. Analysis of phenolic compounds was carried out by headspace solid-phase microextraction (HS-SPME) coupled to gas chromatography-mass spectrometry (GC-MS). Five different fiber coatings were employed in this study. By means of a central composite design, extraction time, salt concentration, and pH of the solution were optimized: 65-{mu}m carbowax-divinylbenzene, extraction time 90 min, concentration in NaCl of 35% (m/v), and pH 2 yielded the highest response. Detection limits of phenol and their alkyl derivatives, guaiacol and eugenol, are between 1.13 and 4.60 ng mL{sup -1}. 3-Methoxyphenol, 2,6-dimethoxyphenol, and vanillin have detection limits considerably higher. Good linearity (R {sup 2}{>=}0.98) was observed for all calibration curves in the established ranges. The reproducibility of the method (RSD, relative standard deviation) was found to oscillate between 7 and 18% (generally close or lower than 10%). (orig.)

  14. Enhancement of sensitivity in the determination of organic trace compounds in complex matrices with liquid chromatography-mass spectrometry (LC-MS)

    International Nuclear Information System (INIS)

    Mascher, D.G.

    2002-05-01

    The PhD-thesis deals with 'enhancement of sensitivity in the determination of organic trace compounds in complex matrices with liquid chromatography-mass spectrometry (LC-MS)'. Almost the most important factor is the enhancement of the ionization yield with Atmospheric Pressure Chemical Ionization (APCI) or Electrospray Ionization (ESI) in LC-MS. Ionization yields of different compounds can vary by a factor of 10000. Three ways to solve this problem of little ionization yield were tried: 1) Modification of the mobile phase in HPLC 2) Chemical modification of the analytes 3) A new type of ionization called Atmospheric Pressure Photo Ionization (APPI). ad 1) By using specific additives to mobile phases ion suppression that might derive from an ion pair reagent that was necessary for chromatography could be omitted. General remarks cannot be done. ad 2) Chemical modification or so called derivatization is well known for UV- and fluorescence-detection for a long period of time. As substances containing nitrogene (e.g. primary, secondary or tertiary amines) often have good ionization yields, poor or relatively poor ionizable substances like carboxylic acids, sugars and partially phenolic steroids were used as analytes for derivatization reactions. By using Dansyl as Dansylchlorid or Dansylhydrazine a basic derivatization agent could be found that ionizes very well. A 200 times more sensitive determination of estrogenes is possible after derivatization with Dansylchlorid. Using a tandem-mass-spectrometer a lower limit of quantification of 2 pg/mL plasma could be reached by using 1 mL of plasma. For ketones like carvon and campher an enhancement by a factor of 500 and 4000 could be reached by using Dansylhydrazine as the derivatization agent. For fatty acids DMEQ as derivatization agent enhanced the sensitivity by a factor of 20 to 100. ad 3) APPI as a new ionization mode showed really good results for specific molecules. Relatively unpolar substances as diphenylsulfide

  15. Analysis of endocrine disruptor compounds in marine sediments by in cell clean up-pressurized liquid extraction-liquid chromatography tandem mass spectrometry determination.

    Science.gov (United States)

    Salgueiro-González, N; Turnes-Carou, I; Muniategui-Lorenzo, S; López-Mahía, P; Prada-Rodríguez, D

    2014-12-10

    A less time-, solvent- and sorbent-consuming analytical methodology for the determination of bisphenol A and alkylphenols (4-tert-octylphenol, 4-octylphenol, 4-n-nonylphenol, nonylphenol) in marine sediment was developed and validated. The method was based on selective pressurized liquid extraction (SPLE) with a simultaneous in cell clean up combined with liquid chromatography-electrospray ionization tandem mass spectrometry in negative mode (LC-ESI-MS/MS). The SPLE extraction conditions were optimized by a Plackett-Burman design followed by a central composite design. Quantitation was performed by standard addition curves in order to correct matrix effects. The analytical features of the method were satisfactory: relative recoveries varied between 94 and 100% and repeatability and intermediate precision were <6% for all compounds. Uncertainty assessment of measurement was estimated on the basis of an in-house validation according to EURACHEM/CITAC guide. Quantitation limits of the method (MQL) ranged between 0.17 (4-n-nonylphenol) and 4.01 ng g(-1) dry weight (nonylphenol). Sensitivity, selectivity, automaticity and fastness are the main advantages of this green methodology. As an application, marine sediment samples from Galicia coast (NW of Spain) were analysed. Nonylphenol and 4-tert-octylphenol were measured in all samples at concentrations between 20.1 and 1409 ng g(-1) dry weight, respectively. Sediment toxicity was estimated and no risk to aquatic biota was found. Copyright © 2014 Elsevier B.V. All rights reserved.

  16. Determination of organotin compounds in waters by headspace solid phase microextraction gas chromatography triple quadrupole tandem mass spectrometry under the European Water Framework Directive.

    Science.gov (United States)

    Moscoso-Pérez, C; Fernández-González, V; Moreda-Piñeiro, J; López-Mahía, P; Muniategui-Lorenzo, S; Prada-Rodríguez, D

    2015-03-13

    The European Union Water Framework Directive (2013/39/EU) sets very restrictive environmental quality standards for 45 priority substances and other pollutants, including organotin compounds (OTCs). Therefore, it is necessary to develop analytical methods in compliance with the environmental quality standard (EQSs) proposed to protect the aquatic environment and humans. The proposed method (HS-SPME-GC-QqQ-MS/MS) allows the determination of OTCs, i.e. monobutyltin (MBT), dibutyltin (DBT) and TBT in water in the range of few ng L(-1). The method is nearly full automated, sensitive and simple; it involves less reagents, reduces waste, and is less-time consuming than traditional methods for OTCs. As such, the procedure connects with the principles of green analytical chemistry. Additionally, good precision (RSD<20%), a very low method quantification limit (MQL) (0.76 ng L(-1) for TBT by using only 10 mL of sample) and excellent linearity (range MQL-20 ng L(-1)) are achieved. Under these conditions, the very restrictive limits for the environmental quality standards (EQS) fixed by the 2013/39/EU Directive are achieved. Copyright © 2015 Elsevier B.V. All rights reserved.

  17. Determination of Optimal Imaging Mode for Ultrasonographic Detection of Subdermal Contraceptive Rods: Comparison of Spatial Compound, Conventional, and Tissue Harmonic Imaging Methods

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Sung Jin; Seo, Kyung; Song, Ho Taek; Park, Ah Young; Kim, Yaena; Yoon, Choon Sik [Gangnam Severance Hospital, Yonsei University College of Medicine, Seoul (Korea, Republic of); Suh, Jin Suck; Kim, Ah Hyun [Dept. of Radiology and Research Institute of Radiological Science, Severance Hospital, Yonsei University College of Medicine, Seoul (Korea, Republic of); Ryu, Jeong Ah [Dept. of Radiology, Guri Hospital, Hanyang University College of Medicine, Guri (Korea, Republic of); Park, Jeong Seon [Dept. of Radiology, Hanyang University Hospital, Hanyang University College of Medicine, Seoul (Korea, Republic of)

    2012-09-15

    To determine which mode of ultrasonography (US), among the conventional, spatial compound, and tissue-harmonic methods, exhibits the best performance for the detection of Implanon with respect to generation of posterior acoustic shadowing (PAS). A total of 21 patients, referred for localization of impalpable Implanon, underwent US, using the three modes with default settings (i.e., wide focal zone). Representative transverse images of the rods, according to each mode for all patients, were obtained. The resulting 63 images were reviewed by four observers. The observers provided a confidence score for the presence of PAS, using a five-point scale ranging from 1 (definitely absent) to 5 (definitely present), with scores of 4 or 5 for PAS being considered as detection. The average scores of PAS, obtained from the three different modes for each observer, were compared using one-way repeated measure ANOVA. The detection rates were compared using a weighted least square method. Statistically, the tissue harmonic mode was significantly superior to the other two modes, when comparing the average scores of PAS for all observers (p < 0.00-1). The detection rate was also highest for the tissue harmonic mode (p < 0.001). Tissue harmonic mode in US appears to be the most suitable in detecting subdermal contraceptive implant rods.

  18. Determination of Optimal Imaging Mode for Ultrasonographic Detection of Subdermal Contraceptive Rods: Comparison of Spatial Compound, Conventional, and Tissue Harmonic Imaging Methods

    International Nuclear Information System (INIS)

    Kim, Sung Jin; Seo, Kyung; Song, Ho Taek; Park, Ah Young; Kim, Yaena; Yoon, Choon Sik; Suh, Jin Suck; Kim, Ah Hyun; Ryu, Jeong Ah; Park, Jeong Seon

    2012-01-01

    To determine which mode of ultrasonography (US), among the conventional, spatial compound, and tissue-harmonic methods, exhibits the best performance for the detection of Implanon with respect to generation of posterior acoustic shadowing (PAS). A total of 21 patients, referred for localization of impalpable Implanon, underwent US, using the three modes with default settings (i.e., wide focal zone). Representative transverse images of the rods, according to each mode for all patients, were obtained. The resulting 63 images were reviewed by four observers. The observers provided a confidence score for the presence of PAS, using a five-point scale ranging from 1 (definitely absent) to 5 (definitely present), with scores of 4 or 5 for PAS being considered as detection. The average scores of PAS, obtained from the three different modes for each observer, were compared using one-way repeated measure ANOVA. The detection rates were compared using a weighted least square method. Statistically, the tissue harmonic mode was significantly superior to the other two modes, when comparing the average scores of PAS for all observers (p < 0.00-1). The detection rate was also highest for the tissue harmonic mode (p < 0.001). Tissue harmonic mode in US appears to be the most suitable in detecting subdermal contraceptive implant rods.

  19. On the magnetism of the C14 Nb0.975Fe2.025 Laves phase compound: Determination of the H-T phase diagram

    Science.gov (United States)

    Bałanda, Maria; Dubiel, Stanisław M.

    2018-05-01

    A C14 Nb0.975Fe2.025 Laves phase compound was investigated aimed at determining the H-T magnetic phase diagram. Magnetization, M, and AC magnetic susceptibility measurement were performed. Concerning the former field-cooled and zero-field-cooled M-curves were recorded in the temperature range of 2-200 K and in applied magnetic field, H, up to 1000 Oe, isothermal M(H) curves at 2 K, 5 K, 50 K, 80 K and 110 K as well as hysteresis loops at several temperatures over the field range of ±10 kOe were measured. Regarding the AC susceptibility, χ, both real and imaginary components were registered as a function of increasing temperature in the interval of 2 K-150 K at the frequencies of the oscillating field, f, from 3 Hz up to 999 Hz. An influence of the external DC magnetic field on the temperature dependence of χ was investigated, too. The measurements clearly demonstrated that the magnetism of the studied sample is weak, itinerant and has a reentrant character. Based on the obtained results a magnetic phase diagram has been constructed in the H-T coordinates.

  20. Simultaneous determination three phytosterol compounds, campesterol, stigmasterol and daucosterol in Artemisia apiacea by high performance liquid chromatography-diode array ultraviolet/visible detector

    Science.gov (United States)

    Lee, Jiwoo; Weon, Jin Bae; Yun, Bo-Ra; Eom, Min Rye; Ma, Choong Je

    2015-01-01

    Background: Artemisia apiacea is a traditional herbal medicine using treatment of eczema and jaundice in Eastern Asia, including China, Korea, and Japan. Objective: An accurate and sensitive analysis method using high performance liquid chromatography-diode array ultraviolet/visible detector and liquid chromatography–mass spectrometry for the simultaneous determination of three phytosterol compounds, campesterol, stigmasterol and daucosterol in A. apiacea was established. Materials and Methods: The analytes were separated on a Shiseido C18 column (5 μm, 4.6 mm I.D. ×250 mm) with gradient elution of 0.1% trifluoroacetic acid and acetonitrile. The flow rate was 1 mL/min and detection wavelengths were set at 205 and 254 nm. Results: Validation of the method was performed to demonstrate its linearity, precision and accuracy. The calibration curves showed good linearity (R2 > 0.9994). The limits of detection and limits of quantification were within the ranges 0.55–7.07 μg/mL and 1.67–21.44 μg/mL, respectively. And, the relative standard deviations of intra- and inter-day precision were <2.93%. The recoveries were found to be in the range of 90.03–104.91%. Conclusion: The developed method has been successfully applied to the analysis for quality control of campesterol, stigmasterol and daucosterol in A. apiacea. PMID:25829768

  1. Evaluation of three analytical techniques used to determine high levels of volatile organic compounds in type IV sludge from Rocky Flats Plant

    International Nuclear Information System (INIS)

    Parish, K.J.; Applegate, D.V.; Tsai, Y.

    1996-01-01

    Before disposal, radioactive sludge (Type IV) from Rocky Flats Plant (RFP) must be evaluated for volatile organic compound (VOC) content. The Type IV sludge consists of organic solvents, degreasers, cutting oils, and transuranic (TRU) waste mixed with calcium silicate (MicroCel E reg-sign) and Oil Dri reg-sign to form a grease or paste-like material. For laboratory testing, a simulated Type IV RFP sludge (nonradioactive) was prepared at Argonne National Laboratory-East. This sludge has a composition similar to that expected from field samples. On the basis of historical information, a typical Type IV sludge is expected to contain approximately 1-10 percent of three target VOCs. The objective of this work is to evaluate three proposed methods for the determination of high levels of these three VOCs in Type IV sludge. The three methods are (1) static headspace gas analysis, (2) methanol extraction, and (3) ethylene glycol extraction. All three methods employ gas chromatography/mass spectrometry (GC/MS). They were evaluated regarding general method performance criteria, ease of operation, and amounts of secondary mixed waste generated

  2. [Determination of di (hydrogenated tallow alkyl) dimethyl ammonium compounds in textile auxiliaries by ultra-high performance liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Zhu, Feng

    2015-01-01

    A method has been developed for the determination of di (hydrogenated tallow alkyl) dimethyl ammonium compounds (DHTDMAC) in textile auxiliaries by ultra-high performance liquid chromatography-tandem mass spectrometry. (UPLC-MS/MS). The samples were extracted and diluted with acidified methanol by 5% (v/v) formic acid under ultrasonic assistance. The separation was performed on an Eclipse Plus C18 column (50 mm x 2.1 mm, 1.8 microm) using 0.1% (v/v) formic acid solution and methanol as the mobile phases. Identification and quantification were achieved by UPLC-MS/MS with electrospray ionization (ESI) source in positive ion mode and multiple reaction monitoring (MRM) mode. The results indicated that the calibration curve of DHTDMAC showed good linear relationship between peak area and mass concentration in the range of 10-280 microg/L with the correlation coefficient (r2) of 0.9991. The limit of detection (LOD, S/N=3) and the limit of quantification (LOQ, S/N= 10) of this method were 3 mg/kg and 10 mg/kg, respectively. The average recoveries from three typical textile auxiliary matrices including dispersant, antistatic agent and fabric softener, at three spiked levels were in the range of 97.2%-108.3% with the relative standard deviations (RSDs) of 1.5%-4.6%. The method is sensitive, accurate, simple and effective for the analysis of DHTDMAC in textile auxiliaries.

  3. Enantioselective column coupled electrophoresis employing large bore capillaries hyphenated with tandem mass spectrometry for ultra-trace determination of chiral compounds in complex real samples.

    Science.gov (United States)

    Piešťanský, Juraj; Maráková, Katarína; Kovaľ, Marián; Havránek, Emil; Mikuš, Peter

    2015-12-01

    A new multidimensional analytical approach for the ultra-trace determination of target chiral compounds in unpretreated complex real samples was developed in this work. The proposed analytical system provided high orthogonality due to on-line combination of three different methods (separation mechanisms), i.e. (1) isotachophoresis (ITP), (2) chiral capillary zone electrophoresis (chiral CZE), and (3) triple quadrupole mass spectrometry (QqQ MS). The ITP step, performed in a large bore capillary (800 μm), was utilized for the effective sample pretreatment (preconcentration and matrix clean-up) in a large injection volume (1-10 μL) enabling to obtain as low as ca. 80 pg/mL limits of detection for the target enantiomers in urine matrices. In the chiral CZE step, the different chiral selectors (neutral, ionizable, and permanently charged cyclodextrins) and buffer systems were tested in terms of enantioselectivity and influence on the MS detection response. The performance parameters of the optimized ITP - chiral CZE-QqQ MS method were evaluated according to the FDA guidance for bioanalytical method validation. Successful validation and application (enantioselective monitoring of renally eliminated pheniramine and its metabolite in human urine) highlighted great potential of this chiral approach in advanced enantioselective biomedical applications. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Multiresponse optimization of a UPLC method for the simultaneous determination of tryptophan and 15 tryptophan-derived compounds using a Box-Behnken design with a desirability function.

    Science.gov (United States)

    Setyaningsih, Widiastuti; Saputro, Irfan E; Carrera, Ceferino A; Palma, Miguel; Barroso, Carmelo G

    2017-06-15

    A Box-Behnken design was used in conjunction with multiresponse optimization based on the desirability function to carry out the simultaneous separation of tryptophan and 15 derivatives by Ultra Performance Liquid Chromatography. The gradient composition of the mobile phase and the flow rate were optimized with respect to the resolution of severely overlapping chromatographic peaks and the total run time. Two different stationary phases were evaluated (hybrid silica and a solid-core-based C 18 column). The methods were validated and a suitable sensitivity was found for all compounds in the concentration range 1-100μgL -1 (R 2 >0.999). High levels of repeatability and intermediate precision (CV less than 0.25% and 1.7% on average for the retention time and the signal area, respectively) were obtained. The new method was applied to the determination tryptophan and its derivatives in black pigmented glutinous and non-glutinous rice grain samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

  5. An integrated evidence-based targeting strategy for determining combinatorial bioactive ingredients of a compound herbal medicine Qishen Yiqi dripping pills.

    Science.gov (United States)

    Zhang, Yiqian; Yu, Jiahui; Zhang, Wen; Wang, Yuewei; He, Yi; Zhou, Shuiping; Fan, Guanwei; Yang, Hua; Zhu, Yan; Li, Ping

    2018-06-12

    Qishen Yiqi is a widely used Chinese herbal medicine formula with "qi invigorating and blood activating" property. Its dripping pill preparation (QSYQ) is a commercial herbal medicine approved by the China Food and Drug Administration (CFDA) in 2003 and is extensively used clinically to treat cardiovascular diseases, such as ischemic heart failure and angina pectoris, as well as for the secondary prevention of myocardial infarction. However, the bioactive ingredients of QSYQ remain unclear. As QSYQ is a compound herbal formula, it is of great importance to elucidate its pharmacologically active ingredients and underlying synergetic effects. This experimental study was conducted to comprehensively determine the combinatorial bioactive ingredients (CBIs) in QSYQ and to elucidate their potential synergetic effects. The established strategy may shed new light on how to rapidly determine CBIs in complex herbal formulas with holistic properties. An integrated evidence-based targeting strategy was introduced and validated to determine CBIs in QSYQ. The strategy included the following steps: (1) Chemical ingredients in QSYQ were analyzed via UPLC-Q-TOF/MS in the negative and positive modes and were identified by comparison with standard compounds and previously reported data. Their potential therapeutic activities were predicted based on the ChEMBL database to preliminarily search for candidate bioactive ingredients, and their combination was defined as the CBIs. (2) The CBIs were directly trapped and prepared from QSYQ with a two-dimensional chromatographic separation system, and the remaining part was defined as the rest ingredients (RIs). (3) As animal and cell models, left anterior descending coronary artery ligation (LAD)-induced heart failure in rats and hypoxia-induced cardiac myocyte injury in H9c2 cells were applied to compare the potency of QSYQ, CBIs and RIs. (4) The synergetic effects on cardiac myocyte protection of multiple ingredients in CBIs were examined

  6. Development and application of radioimmunological methods to determine an anabolic compound (trenboloneacetate sup(R)) and its major metabolite (trenbolone) in various tissues and in bovine plasma

    International Nuclear Information System (INIS)

    Oettel, G.M.

    1976-01-01

    For quantitation of the anabolic compound trenboloneacetate sup(R)(TBA) and its major metabolite trenbolone (TBOH) a radioimmunoassay (RIA) was established after raising antibodies in rabbits immunized with TBA-3-(o-carboxi-methyl)-oxime-BSA and TBOH-17β-hemisuccinate-BSA. In order to apply this assay for residue determinations in muscle, liver kidney and fat as well as in plasma of treated animals specific extraction procedures were developed. Specifity, sensitivity, accuracy and reproductibility were tested and the developed methods were shown to be highly reliable. Besides free also conjugated TBOH could be determined after enzyme hydrolysis. The lower limit of sensitivity was around 45 pg; at present 100 tissue samples can be analyzed by one person during one week. With the methods described tissue and plasma samples of 41 heifer calves, 10 bull calves and two steers were analyzed for residues of TBA and TBOH. The animals were treated with various dosages of TBA, alone or in combination with oestradiol-17β. In treated animals the highest residue levels were found in liver, with conjugated TBOH being the major residue fraction (76,4%). Second ranking after liver were fat and kidney tissue with similarly high total residue concentrations, however, free TBOH being the major residue fraction (84,1%) in fat, while each, free and conjugated TBOH, accounted for about 50% in kidney. Lowest residue concentrations with free TBOH being the major residue fraction (91,5%) were found in general in muscular tissue. TBA could only be quantitated in fat (14.2% of total residues). (orig.) [de

  7. Utilizing a CdTe quantum dots-enzyme hybrid system for the determination of both phenolic compounds and hydrogen peroxide.

    Science.gov (United States)

    Yuan, Jipei; Guo, Weiwei; Wang, Erkang

    2008-02-15

    In this paper, we attempt to construct a simple and sensitive detection method for both phenolic compounds and hydrogen peroxide, with the successful combination of the unique property of quantum dots and the specificity of enzymatic reactions. In the presence of H2O2 and horseradish peroxidase, phenolic compounds can quench quantum dots' photoluminescence efficiently, and the extent of quenching is severalfold to more than 100-fold increase. Quinone intermediates produced from the enzymatic catalyzed oxidation of phenolic compounds were believed to play the main role in the photoluminescence quenching. Using a quantum dots-enzyme system, the detection limits for phenolic compounds and hydrogen peroxide were detected to be approximately 10(-7) mol L(-1). The coupling of efficient quenching of quantum dot photoluminescence by quinone and the effective enzymatic reactions make this a simple and sensitive method for phenolic compound detection and great potential in the development of H2O2 biosensors for various analytes.

  8. Simultaneous multi-species determination of trimethyllead, monomethylmercury and three butyltin compounds by species-specific isotope dilution GC-ICP-MS in biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Poperechna, Nataliya; Heumann, Klaus G. [Johannes Gutenberg-University Mainz (Germany). Institute of Inorganic Chemistry and Analytical Chemistry

    2005-09-01

    An accurate and sensitive multi-species species-specific isotope dilution GC-ICP-MS method was developed for the simultaneous determination of trimethyllead (Me{sub 3}Pb{sup +}), monomethylmercury (MeHg{sup +}) and the three butyltin species Bu{sub 3}Sn{sup +}, Bu{sub 2}Sn{sup 2+}, and BuSn{sup 3+} in biological samples. The method was validated by three biological reference materials (CRM 477, mussel tissue certified for butyltins; CRM 463, tuna fish certified for MeHg{sup +}; DORM 2, dogfish muscle certified for MeHg{sup +}). Under certain conditions, and with minor modifications of the sample pretreatment procedure, this method could also be transferred to environmental samples such as sediments, as demonstrated by analyzing sediment reference material BCR 646 (freshwater sediment, certified for butyltins). The detection limits of the multi-species GC-ICP-IDMS method for biological samples were 1.4 ng g{sup -1} for MeHg{sup +}, 0.06 ng g{sup -1} for Me{sub 3}Pb{sup +}, 0.3 ng g{sup -1} for BuSn{sup 3+} and Bu{sub 3}Sn{sup +}, and 1.2 ng g{sup -1} for Bu{sub 2}Sn{sup 2+}. Because of the high relevance of these heavy metal alkyl species to the quality assurance of seafood, the method was also applied to corresponding samples purchased from a supermarket. The methylated lead fraction in these samples, correlated to total lead, varied over a broad range (from 0.01% to 7.6%). On the other hand, the MeHg{sup +} fraction was much higher, normally in the range of 80-100%. Considering that we may expect tighter legislative limitations on MeHg{sup +} levels in seafood in the future, we found the highest methylmercury contents (up to 10.6 {mu}g g{sup -1}) in two shark samples, an animal which is at the end of the marine food chain, whereas MeHg{sup +} contents of less than 0.2 {mu}g g{sup -1} were found in most other seafood samples; these results correlate with the idea that MeHg{sup +} is usually of biological origin in the marine environment. The concentration of

  9. Determination of anthropogenic and biogenic compounds on atmospheric aerosol collected in urban, biomass burning and forest areas in São Paulo, Brazil.

    Science.gov (United States)

    Vasconcellos, Pérola C; Souza, Davi Z; Sanchez-Ccoyllo, Odon; Bustillos, José Oscar V; Lee, Helena; Santos, Fernando C; Nascimento, Katia H; Araújo, Maria P; Saarnio, Karri; Teinilä, Kimmo; Hillamo, Risto

    2010-11-01

    This study was conducted at three sites of different characteristics in São Paulo State: São Paulo (SPA), Piracicaba (PRB) and Mata Atlântica Forest (MAT). PM(10), n-alkanes, pristane and phytane, PAHs, water-soluble ions and biomass burning tracers like levoglucosan and retene, were determined in quartz fiber filters. Samplings occurred on May 8th to August 8th, 2007 at the MAT site; on August 15th to 29th in 2007 and November 10th to 29th in 2008 at the PRB site and, March 13th to April 4th in 2007 and August 7th to 29th in 2008 at the SPA site. Aliphatic compounds emitted biogenically were less abundant at the urban sites than at the forest site, and its distribution showed the influence of tropical vascular plants. Air mass transport from biomass burning regions is likely to impact the sites with specific molecular markers. The concentrations of all species were variable and dependent of seasonal changes. In the most dry and polluted seasons, n-alkane and cation total concentrations were similar between the megacity and the biomass burning site. PAHs and inorganic ion abundances were higher at São Paulo than Piracicaba, yet, the site influenced by biomass burning seems to be the most impacted by the organic anion abundance in the atmosphere. Pristane and phytane confirm the contamination by petroleum residues at urban sites; at the MAT site, biological activity and long range transport of pollutants might influence the levels of pristane. Copyright © 2010 Elsevier B.V. All rights reserved.

  10. Retroconversion is a minor contributor to increases in eicosapentaenoic acid following docosahexaenoic acid feeding as determined by compound specific isotope analysis in rat liver.

    Science.gov (United States)

    Metherel, Adam H; Chouinard-Watkins, Raphaël; Trépanier, Marc-Olivier; Lacombe, R J Scott; Bazinet, Richard P

    2017-01-01

    Dietary docosahexaenoic acid (DHA, 22:6n-3) not only increases blood and tissue levels of DHA, but also eicosapentaenoic acid (EPA, 20:5n-3). It is generally believed that this increase is due to DHA retroconversion to EPA, however, a slower conversion of α-linolenic acid (ALA, 18:3n-3) derived EPA to downstream metabolic products (i.e. slower turnover of EPA) is equally plausible. In this study, 21-day old Long Evans rats were weaned onto an ALA only or DHA + ALA diet for 12 weeks. Afterwards, livers were collected and the natural abundance 13 C-enrichment was determined by compound specific isotope analysis (CSIA) of liver EPA by isotope ratio mass-spectrometry and compared to dietary ALA and DHA 13 C-enrichment. Isotopic signatures (per mil, ‰) for liver EPA were not different ( p  > 0.05) between the ALA only diet (-25.89 ± 0.39 ‰, mean ± SEM) and the DHA + ALA diet (-26.26 ± 0.40 ‰), suggesting the relative contribution from dietary ALA and DHA to liver EPA did not change. However, with DHA feeding estimates of absolute EPA contribution from ALA increased 4.4-fold (147 ± 22 to 788 ± 153 nmol/g) compared to 3.2-fold from DHA (91 ± 14 to 382 ± 13 nmol/g), respectively. In conclusion, CSIA of liver EPA in rats following 12-weeks of dietary DHA suggests that retroconversion of DHA to EPA is a relatively small contributor to increases in EPA, and that this increase in EPA is largely coming from elongation/desaturation of ALA.

  11. Fabrication of new carbon paste electrodes based on gold nano-particles self-assembled to mercapto compounds as suitable ionophores for potentiometric determination of copper ions

    Directory of Open Access Journals (Sweden)

    Rasoul Pourtaghavi Talemi

    2013-12-01

    Full Text Available In the present study, we investigate the potentiometric behavior of Cu2+ carbon paste electrodes based on two mercapto compounds 2-ethylmino-5-mercapto-1,3,4-thiadiazole (EAMT and 2-acetylamino-5-mercapto-1,3,4-thiadiazole (AAMT self-assembled on gold nano-paricle (GNP as ionophore. Then, the obtained results from the modified electrodes are compared. The self-assembled ionophores exhibit a high selectivity for copper ion (Cu2+, in which the sulfur and nitrogen atoms in their structure play a significant role as the effective coordination donor site for the copper ion. Among these electrodes, the best performance was obtained with the sensor with a EAMT/graphite powder/paraffin oil weight ratio of 4.0/68/28 with 200 µL of GNP which exhibits the working concentration range of 1.6×10−9 to 6.3×10−2 M and a nernstian slope of 28.9±0.4 mVdecade−1 of copper(II activity. The detection limit of electrode was 2.9(±0.2×10−10M and potential response was pH ; in other words, it was independent across the range of 2.8–6.3. The proposed electrode presented very good selectivity and sensitivity towards the Cu2+ ions over a wide variety of cations including alkali, alkaline earth, transition and heavy metal ions. Moreover, the proposed electrode was successfully applied as an indicator electrode in the potentiometric titration of Cu(II ions with EDTA and also the potentiometric determination of copper ions in spiked water samples.

  12. Surface emission determination of volatile organic compounds (VOC) from a closed industrial waste landfill using a self-designed static flux chamber.

    Science.gov (United States)

    Gallego, E; Perales, J F; Roca, F J; Guardino, X

    2014-02-01

    Closed landfills can be a source of VOC and odorous nuisances to their atmospheric surroundings. A self-designed cylindrical air flux chamber was used to measure VOC surface emissions in a closed industrial landfill located in Cerdanyola del Vallès, Catalonia, Spain. The two main objectives of the study were the evaluation of the performance of the chamber setup in typical measurement conditions and the determination of the emission rates of 60 different VOC from that industrial landfill, generating a valuable database that can be useful in future studies related to industrial landfill management. Triplicate samples were taken in five selected sampling points. VOC were sampled dynamically using multi-sorbent bed tubes (Carbotrap, Carbopack X, Carboxen 569) connected to SKC AirCheck 2000 pumps. The analysis was performed by automatic thermal desorption coupled with a capillary gas chromatograph/mass spectrometry detector. The emission rates of sixty VOC were calculated for each sampling point in an effort to characterize surface emissions. To calculate average, minimum and maximum emission values for each VOC, the results were analyzed by three different methods: Global, Kriging and Tributary area. Global and Tributary area methodologies presented similar values, with total VOC emissions of 237 ± 48 and 222 ± 46 g day(-1), respectively; however, Kriging values were lower, 77 ± 17 gd ay(-1). The main contributors to the total emission rate were aldehydes (nonanal and decanal), acetic acid, ketones (acetone), aromatic hydrocarbons and alcohols. Most aromatic hydrocarbon (except benzene, naphthalene and methylnaphthalenes) and aldehyde emission rates exhibited strong correlations with the rest of VOC of their family, indicating a possible common source of these compounds. B:T ratio obtained from the emission rates of the studied landfill suggested that the factors that regulate aromatic hydrocarbon distributions in the landfill emissions are different from the ones

  13. Optimization of the HS-SPME-GC/MS technique for determining volatile compounds in red wines made from Isabel grapes (Vitis labrusca

    Directory of Open Access Journals (Sweden)

    Narciza Maria de Oliveira ARCANJO

    2015-01-01

    Full Text Available AbstractBrazilian wine production is characterized by Vitis labrusca grape varieties, especially the economically important Isabel cultivar, with over 80% of its production destined for table wine production. The objective of this study was to optimize and validate the conditions for extracting volatile compounds from wine with the solid-phase microextraction technique, using the response surface method. Based on the response surface analysis, it can be concluded that the central point values maximize the process of extracting volatile compounds from wine, i.e., an equilibrium time of 15 minutes, an extraction time of 35 minutes, and an extraction temperature of 30 °C. Esters were the most numerous compounds found under these extraction conditions, indicating that wines made from Isabel cultivar grapes are characterized by compounds that confer a fruity aroma; this finding corroborates the scientific literature.

  14. The Efficient Extraction of Phenolic Compounds from Oak Gall Using a Miniaturized Matrix Solid-Phase Dispersion Method before their HPLC Determination

    Directory of Open Access Journals (Sweden)

    Ahmad Daneshfar

    2017-06-01

    Conclusion: The proposed technique is simple and fast. It substantially reduced the amounts of sample, sorbent and organic solvents required for the extraction. The maximum amounts of the phenolic compounds were found in Qalqaf and Bramazu galls.

  15. Anti-methicillin Resistant Staphylococcus aureus Compound Isolation from Halophilic Bacillus amyloliquefaciens MHB1 and Determination of Its Mode of Action Using Electron Microscope and Flow Cytometry Analysis

    OpenAIRE

    Jeyanthi, Venkadapathi; Velusamy, Palaniyandi

    2016-01-01

    The aim of this study was to purify, characterize and evaluate the antibacterial activity of bioactive compound against methicillin-resistant Staphylococcus aureus (MRSA). The anti-MRSA compound was produced by a halophilic bacterial strain designated as MHB1. The MHB1 strain exhibited 99��% similarity to Bacillus amyloliquefaciens based on 16S rRNA gene analysis. The culture conditions of Bacillus amyloliquefaciens MHB1 were optimized using nutritional and environmental parameters for enhanc...

  16. Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory - Determination of Wastewater Compounds by Polystyrene-Divinylbenzene Solid-Phase Extraction and Capillary-Column Gas Chromatography/Mass Spectrometry

    Science.gov (United States)

    Zaugg, Steven D.; Smith, Steven G.; Schroeder, Michael P.; Barber, Larry B.; Burkhardt, Mark R.

    2002-01-01

    A method for the determination of 67 compounds typically found in domestic and industrial wastewater is described. The method was developed in response to increasing concern over the impact of endocrine-disrupting chemicals in wastewater on aquatic organisms. This method also may be useful for evaluating the impact of combined sanitary and storm-sewer overflow on the water quality of urban streams. The method focuses on the determination of compounds that are an indicator of wastewater or that have been chosen on the basis of their endocrine-disrupting potential or toxicity. These compounds include the alkylphenol ethoxylate nonionic surfactants and their degradates, food additives, fragrances, antioxidants, flame retardants, plasticizers, industrial solvents, disinfectants, fecal sterols, polycyclicaromatic hydrocarbons, and high-use domestic pesticides. Water samples are filtered to remove suspended particulate matter and then are extracted by vacuum through disposable solid-phase cartridges that contain polystyrene-divinylbenzene resin. Cartridges are dried with nitrogen gas, and then sorbed compounds are eluted with dichloromethane-diethyl ether (4:1) and determined by capillary-column gas chromatography/mass spectrometry. Recoveries in reagent-water samples fortified at 4 micrograms per liter averaged 74 percent ? 7 percent relative standard deviation for all method compounds. Initial method detection limits for single-component compounds (excluding hormones and sterols) averaged 0.15 microgram per liter. Samples are preserved by filtration, the addition of 60 grams NaCl, and storage at 4 degrees Celsius. The laboratory has established a sample-holding time (prior to sample extraction) of 14 days from the date of sample collection until a statistically accepted method can be used to determine the effectiveness of these sample-preservation procedures.

  17. Hybridization in Kondo lattice heavy fermions via quasiparticle scattering spectroscopy (QPS)

    Science.gov (United States)

    Narasiwodeyar, Sanjay; Dwyer, Matt; Greene, Laura; Park, Wan Kyu; Bauer, Eric; Tobash, Paul; Baumbach, Ryan; Ronning, Filip; Sarrao, John; Thompson, Joe; Canfield, Paul

    2014-03-01

    Band renormalization in a Kondo lattice via hybridization of the conduction band with localized states has been a hot topic over the last several years. In part, this has to do with recently reignited interest in the hidden order problem in URu2Si2. Despite recent developments regarding the electronic structure in this compound, it remains to be resolved whether the hidden order phase transition is related to the opening of a hybridization gap. Our quasiparticle scattering spectroscopy (QPS) has shown they are not related directly. This can be understood naturally since in principle band renormalization does not involve symmetry breaking. To deepen our understanding, we extend to other Kondo lattice compounds. For instance, when applied to YbAl3, a vegetable heavy-fermion system, QPS reveals conductance signatures for hybridization in a Kondo lattice such as asymmetric Fano background along with characteristic energy scales. Presenting new results on these materials, we will discuss a broader picture. The work at UIUC is supported by the NSF DMR 12-06766, the work at LANL is carried out under the auspices of the U.S. DOE, Office of Science, and the work done at Ames Lab. was supported under Contract No. DE-AC02-07CH11358.

  18. Simultaneous determination of various aromatic amines and metabolites of aromatic nitro compounds in urine for low level exposure using gas chromatography-mass spectrometry.

    Science.gov (United States)

    Weiss, Tobias; Angerer, Jürgen

    2002-10-05

    A newly developed method permits the simultaneous quantitative determination of various aromatic amines (or metabolites of aromatic nitro compounds, respectively) in human urine in one analytical run. Applying this method it is possible to determine aniline, toluidines, 4-isopropylaniline, o-anisidine, 3- and 4-chloroaniline, 4-bromoaniline, aminonitrotoluenes, aminodinitrotoluenes, 3,5- and 3,4-dichloroaniline, alpha- and beta-naphtylamine and 4-aminodiphenyl. After separation from the urinary matrix by a simple liquid-liquid extraction at pH 6.2-6.4 the analytes are converted into their pentafluoropropionic acid amides. Separation and quantitative analysis is carried out by capillary gas chromatography and mass-selective detection in the single ion monitoring mode. The limits of detection were within the range from 0.05 microg/l (4-aminobiphenyl, o-anisidine, 3,5-dichloroaniline) to 2 microg/l urine (4-amino-2,6-dinitrotoluene). The relative standard deviation of the within-series imprecision (determined at spiked concentrations of 2.0 microg/l and 10 microg/l) was between 2.9 and 13.6% depending on analyte and concentration. The relative recovery rates were in the range of 70-121%. The analytes that do not contain a nitro function showed better performance regarding the analytical reliability criteria. In order to determine the suitability of this new method for biological monitoring we analysed 20 12-h urine samples of persons without known exposure to aromatic amines, nitroaromatics or precursors in a pilot study. In these samples various aromatic amines could be clearly identified. The general population renally excretes aniline (median: 3.5 microg/l; 95th percentile: 7.9 microg/l), o- (0.12 microg/l; 2.7 microg/l), m- (0.17 microg/l; 2.2 microg/l) and p-toluidine (0.11 microg/l; 0.43 microg/l), and o-anisidine (0.22 microg/l; 0.68 microg/l). Additionally, we found that the persons investigated also excrete 3- (<0.05 microg/l; 0.55 microg/l) and 4

  19. Simultaneous determination of phenolic compounds in Cynthiana grape (Vitis aestivalis) by high performance liquid chromatography-electrospray ionisation-mass spectrometry.

    Science.gov (United States)

    Ramirez-Lopez, L M; McGlynn, W; Goad, C L; Mireles Dewitt, C A

    2014-04-15

    Phenolic acids, flavanols, flavonols and stilbenes (PAFFS) were isolated from whole grapes, juice, or pomace and purified using enzymatic hydrolysis. Only anthocyanin mono-glucosides and a few of the oligomers from Cynthiana grape (Vitis aestivalis) were analysed. Flavonoid-anthocyanin mono-glucosides (FA) were isolated using methanol/0.1% hydrochloric acid extraction. In addition, crude extractions of phenolic compounds from Cynthiana grape using 50% methanol, 70% methanol, 50% acetone, 0.01% pectinase, or petroleum ether were also evaluated. Reverse phase high performance liquid chromatography (RP-HPLC) with photodiode array (PDA) detector was used to identify phenolic compounds. A method was developed for simultaneous separation, identification and quantification of both PAFFS and FA. Quantification was performed by the internal standard method using a five points regression graph of the UV-visible absorption data collected at the wavelength of maximum absorbance for each analyte. From whole grape samples nine phenolic compounds were tentatively identified and quantified. The individual phenolic compounds content varied from 3 to 875 mg kg⁻¹ dry weight. For juice, twelve phenolic compounds were identified and quantified. The content varied from 0.07 to 910 mg kg⁻¹ dry weight. For pomace, a total of fifteen phenolic compounds were tentatively identified and quantified. The content varied from 2 mg kg⁻¹ to 198 mg kg⁻¹ dry matter. Results from HPLC analysis of the samples showed that gallic acid and (+)-catechin hydrate were the major phenolic compounds in both whole grapes and pomace. Cyanidin and petunidin 3-O-glucoside were the major anthocyanin glucosides in the juice. Published by Elsevier Ltd.

  20. Simultaneous determination of phenolic compounds and saponins in quinoa (Chenopodium quinoa Willd) by a liquid chromatography-diode array detection-electrospray ionization-time-of-flight mass spectrometry methodology.

    Science.gov (United States)

    Gómez-Caravaca, Ana María; Segura-Carretero, Antonio; Fernández-Gutiérrez, Alberto; Caboni, Maria Fiorenza

    2011-10-26

    A new liquid chromatography methodology coupled to a diode array detector and a time-of-flight mass spectrometer has been developed for the simultaneous determination of phenolic compounds and saponins in quinoa (Chenopodium quinoa Willd). This method has allowed the simultaneous determination of these two families of compounds with the same analytical method for the first time. A fused-core column C18 has been used, and the analysis has been performed in less than 27 min. Both chromatographic and electrospray ionization time-of-flight mass spectrometry parameters have been optimized to improve the sensitivity and to maximize the number of compounds detected. A validation of the method has also been carried out, and free and bound polar fractions of quinoa have been studied. Twenty-five compounds have been tentatively identified and quantified in the free polar fraction, while five compounds have been tentatively identified and quantified in the bound polar fraction. It is important to highlight that 1-O-galloyl-β-D-glucoside, acacetin, protocatechuic acid 4-O-glucoside, penstebioside, ethyl-m-digallate, (epi)-gallocatechin, and canthoside have been tentatively identified for the first time in quinoa. Free phenolic compounds have been found to be in the range of 2.746-3.803 g/kg of quinoa, while bound phenolic compounds were present in a concentration that varies from 0.139 and 0.164 g/kg. Indeed, saponins have been found to be in a concentration that ranged from 5.6 to 7.5% of the total composition of whole quinoa flour.

  1. Evaluation of the Stability of Mercaptopurine Suspension Compounded in a Commercial Vehicle and the Determination of an Appropriate Beyond-use Date.

    Science.gov (United States)

    Peacock, Gina F; Sauvageot, Jurgita; Hill, Ashley; Killian, Alyssa

    2016-01-01

    Mercaptopurine is commonly used to treat acute lymphoblastic leukemia and has historically been commercially available only in tablet form. Since tablets may be difficult for children and elderly patients to swallow, many pharmacists have compounded mercaptopurine suspensions. The U.S. Food and Drug Administration recently approved a commercial suspension, but it is not widely available at this time. Therefore, pharmacists may still need to compound mercaptopurine suspension for use in areas where it is not available or if the commercial suspension is in short supply. Stability studies must be conducted in order to assign appropriate beyond-use dates for compounded preparations. The objective of this study was to evaluate the stability of extemporaneously compounded suspensions using commercially available mercaptopurine tablets, as well as active pharmaceutical ingredient in a vehicle of Ora-Sweet and Ora-Plus (1:1) stored in plastic and glass containers at room temperature. Each mercaptopurine preparation was analyzed using a validated stability-indicating high-performance liquid chromatography method at the following time points: 0, 7, 14, 21, 30, 60, and 90 days. Suspensions were also observed for changes in appearance or odor, and pH was tested at each time point. The suspension compounded from Roxane generic tablets was extremely viscous and was therefore eliminated from the study. All other suspensions showed no observed physical changes and maintained greater than 93% of initial concentration of mercaptopurine for the entire study period.

  2. Determining

    Directory of Open Access Journals (Sweden)

    Bahram Andarzian

    2015-06-01

    Full Text Available Wheat production in the south of Khuzestan, Iran is constrained by heat stress for late sowing dates. For optimization of yield, sowing at the appropriate time to fit the cultivar maturity length and growing season is critical. Crop models could be used to determine optimum sowing window for a locality. The objectives of this study were to evaluate the Cropping System Model (CSM-CERES-Wheat for its ability to simulate growth, development, grain yield of wheat in the tropical regions of Iran, and to study the impact of different sowing dates on wheat performance. The genetic coefficients of cultivar Chamran were calibrated for the CSM-CERES-Wheat model and crop model performance was evaluated with experimental data. Wheat cultivar Chamran was sown on different dates, ranging from 5 November to 9 January during 5 years of field experiments that were conducted in the Khuzestan province, Iran, under full and deficit irrigation conditions. The model was run for 8 sowing dates starting on 25 October and repeated every 10 days until 5 January using long-term historical weather data from the Ahvaz, Behbehan, Dezful and Izeh locations. The seasonal analysis program of DSSAT was used to determine the optimum sowing window for different locations as well. Evaluation with the experimental data showed that performance of the model was reasonable as indicated by fairly accurate simulation of crop phenology, biomass accumulation and grain yield against measured data. The normalized RMSE were 3%, 2%, 11.8%, and 3.4% for anthesis date, maturity date, grain yield and biomass, respectively. Optimum sowing window was different among locations. It was opened and closed on 5 November and 5 December for Ahvaz; 5 November and 15 December for Behbehan and Dezful;and 1 November and 15 December for Izeh, respectively. CERES-Wheat model could be used as a tool to evaluate the effect of sowing date on wheat performance in Khuzestan conditions. Further model evaluations

  3. Detection of hormonal anabolic compounds in calf urine and unverified growth-promoting preparations : application of the AR-LUX bioassay for screening and determination of androgenic activity

    NARCIS (Netherlands)

    Blankvoort, B.M.G.; Aarts, J.M.M.J.G.; Schilt, R.; Geerdink, P.; Spenkelink, B.; Rodenburg, R.J.T.

    2003-01-01

    Despite a ban by the European Union, the use of anabolic steroids and repartitioning agents in cattle is still occasionally observed. Due to continuing improvements in analytical techniques, very low detection limits for individual compounds have been achieved. In response to these developments,

  4. Detection of hormonal anabolic compounds in calf urine and unverified growth-promoting preparations: application of the AR-LUX bioassay for screening and determination of androgenic activity

    NARCIS (Netherlands)

    Blankvoort, B.M.G.; Aarts, J.M.M.J.G.; Schilt, R.; Geerdink, P.; Spenkelink, A.; Rodenburg, R.J.T.

    2003-01-01

    Despite a ban by the European Union, the use of anabolic steroids and repartitioning agents in cattle is still occasionally observed. Due to continuing improvements in analytical techniques, very low detection limits for individual compounds have been achieved. In response to these developments,

  5. Determination of the levels of dioxin and dioxin-like compounds in the Australian population by analysis of pooled human breast milk

    Energy Technology Data Exchange (ETDEWEB)

    Harden, F.; Mueller, J.F.; Toms, L.M.L.; Moore, M. [National Research Centre for Environmental Toxicology, The Univ. of Queensland, Brisbane (Australia); Burniston, D.; Symons, R. [AGAL, Sydney (Australia); Ahokas, J. [RMIT, Melbourne (Australia); Fuerst, P. [State Lab. of NRW, Muenster (Germany); Paepke, O. [ERGO Forschungsgesellschaft, Hamburg (Germany)

    2004-09-15

    Dioxin-like compounds are ubiquitously distributed and humans are exposed to them via various sources but primarily through food. They can be detected in air, water, soil, sediment and biota. These compounds are lipid soluble, poorly eliminated and thus can accumulate in human adipose tissue. They can cross the placenta and are also transferred to breast milk during the lactation process. Therefore infants are exposed ante and postnatally. Since PCDD/PCDF concentration in blood and human milk are very similar when concentrations are expressed on a lipid basis, human milk provides a good monitoring tool of exposure for a given population in a given area. Previously the WHO has co-ordinated international studies on dioxin-like compounds in breast milk. These were conducted in 1987/88, 1992/93 and 2001. In summary, these studies demonstrated that levels of dioxins in breast milk are relatively high in industrialised countries when compared to non-industrialised countries that PCDD/PCDFs were higher in human milk from mothers with their first child and that the levels decrease over a given lactation period. The present study aims to examine the levels of these compounds in primiparae women throughout Australia.

  6. Determination of isobaric thermal expansivity of organic compounds from 0.1 to 30 MPa at 30 degrees C with an isothermal pressure scanning microcalorimeter

    DEFF Research Database (Denmark)

    Verdier, Sylvain Charles Roland; Andersen, Simon Ivar

    2003-01-01

    This paper describes a simple high-pressure mercury-free microcalorimetric technique that enables the compression of a fluid from 0.1 to 30 MPa. Thermal expansivities of several compounds were calculated (n-hexane, cyclohexane, heptane, and toluene) with the pressure. scanning transitiometry method...

  7. Novel Anthra[1,2-c][1,2,5]Thiadiazole-6,11-Diones as Promising Anticancer Lead Compounds: Biological Evaluation, Characterization & Molecular Targets Determination.

    Directory of Open Access Journals (Sweden)

    Ahmed Atef Ahmed Ali

    Full Text Available The novel compounds NSC745885 and NSC757963 developed at our laboratory were tested against a panel of 60 cancer cell lines at the National Cancer Institute, USA, and a panel of 39 cancer cell lines at the Japanese Foundation of Cancer Research. Both compounds demonstrated selective unique multi-log differential patterns of activity, with GI50 values in the sub-micro molar range against cancer cells rather than normal cardiac cells. NSC757963 showed high selectivity towards the leukemia subpanel. Activities of both compounds strongly correlated to expression of NFKB1 and CSNK2B genes, implying that they may inhibit the NF-κB pathway. Immunocytochemical microscopy of OVCAR-3 cells showed clear cytosolic accumulation of the NF-κB p65 subunit following treatment. Western blotting showed dose dependent inhibition of the nuclear expression of the NF-κB p65 subunit with subsequent accumulation in the cytosol following treatment. Docking experiments showed binding of both compounds to the NF-κB activator IKKβ subunit preventing its translocation to the nucleus. Collectively, these results confirm the ability of our compounds to inhibit the constitutively active NF-κB pathway of OVCAR-3 cells. Furthermore, COMPARE analysis indicated that the activity of NSC757963 is similar to the antituberculosis agent rifamycin SV, this was confirmed by testing the antimycobacterial activity of NSC757963 against Mycobacterium tuberculosis, results revealed potent activity suitable for use in clinical practice. Molecular properties and Lipinski's parameters predicted acceptable bioavailability properties with no indication of mutagenicity, tumorigenicity, irritability and reproductive effects. Oral absorption experiments using the human Caco-2 model showed high intestinal absorption of NSC745885 by passive transport mechanism with no intestinal efflux or active transport mechanisms. The unique molecular characterization as well as the illustrated anticancer

  8. Multipurpose Compound

    Science.gov (United States)

    1983-01-01

    Specially formulated derivatives of an unusual basic compound known as Alcide may be the answer to effective treatment and prevention of the disease bovine mastitis, a bacterial inflammation of a cow's mammary gland that results in loss of milk production and in extreme cases, death. Manufactured by Alcide Corporation the Alcide compound has killed all tested bacteria, virus and fungi, shortly after contact, with minimal toxic effects on humans or animals. Alcide Corporation credits the existence of the mastitis treatment/prevention products to assistance provided the company by NERAC, Inc.

  9. Quantum corrections for the phase diagram of systems with competing order

    Science.gov (United States)

    Silva, N. L., Jr.; Continentino, Mucio A.; Barci, Daniel G.

    2018-06-01

    We use the effective potential method of quantum field theory to obtain the quantum corrections to the zero temperature phase diagram of systems with competing order parameters. We are particularly interested in two different scenarios: regions of the phase diagram where there is a bicritical point, at which both phases vanish continuously, and the case where both phases coexist homogeneously. We consider different types of couplings between the order parameters, including a bilinear one. This kind of coupling breaks time-reversal symmetry and it is only allowed if both order parameters transform according to the same irreducible representation. This occurs in many physical systems of actual interest like competing spin density waves, different types of orbital antiferromagnetism, elastic instabilities of crystal lattices, vortices in a multigap SC and also applies to describe the unusual magnetism of the heavy fermion compound URu2Si2. Our results show that quantum corrections have an important effect on the phase diagram of systems with competing orders.

  10. Superconductivity: Is there a problem in transuranics?

    International Nuclear Information System (INIS)

    Colineau, Eric; Griveau, Jean-Christophe; Eloirdi, Rachel; Hen, Amir; Caciuffo, Roberto

    2014-01-01

    Superconductivity was first reported in 1942 for uranium metal (¡-U) and in 1958 for U compounds: UCo, U6Mn, U6Fe, and U6Co, with critical temperatures Tc, of 1.7, 2.3, 3.9, and 2.3K, respectively. A new class of U superconductors emerged in the early 1980’s with the discovery of U heavy fermion superconductors : UBe13 (Tc = 0.85K), UPt3 (Tc = 0.53K), URu2Si2 (Tc = 1.5K) , UPd2Al3 (Tc = 1.9K) … Furthermore, in most of these systems, the superconducting phases coexist with antiferromagnetic (AF) correlations which have characteristic temperatures, usually the Néel temperature TN, that are typically one order of magnitude greater than the corresponding superconducting critical temperatures Tc. Superconductivity was even shown to co-exist with ferromagnetism in e.g. UGe2 (Tc ï» 0.8K, TC ï» 30K at p ï» 1.2GPa) and URhGe (Tc = 0.25K, TC = 9.5K). Heavy fermion superconductors still remain a major challenge for condensed matter physics. The existence of heavy fermion superconductivity and its coexistence or proximity with magnetic order suggests that the conventional mechanism of phonon-mediated superconductivity is inappropriate and that alternative mechanisms, like spin fluctuations, should be considered for Cooper pairing

  11. Quantum corrections for the phase diagram of systems with competing order.

    Science.gov (United States)

    Silva, N L; Continentino, Mucio A; Barci, Daniel G

    2018-06-06

    We use the effective potential method of quantum field theory to obtain the quantum corrections to the zero temperature phase diagram of systems with competing order parameters. We are particularly interested in two different scenarios: regions of the phase diagram where there is a bicritical point, at which both phases vanish continuously, and the case where both phases coexist homogeneously. We consider different types of couplings between the order parameters, including a bilinear one. This kind of coupling breaks time-reversal symmetry and it is only allowed if both order parameters transform according to the same irreducible representation. This occurs in many physical systems of actual interest like competing spin density waves, different types of orbital antiferromagnetism, elastic instabilities of crystal lattices, vortices in a multigap SC and also applies to describe the unusual magnetism of the heavy fermion compound URu 2 Si 2 . Our results show that quantum corrections have an important effect on the phase diagram of systems with competing orders.

  12. Polymer compound

    NARCIS (Netherlands)

    1995-01-01

    A Polymer compound comprising a polymer (a) that contains cyclic imidesgroups and a polymer (b) that contains monomer groups with a 2,4-diamino-1,3,5-triazine side group. According to the formula (see formula) whereby themole percentage ratio of the cyclic imides groups in the polymer compoundwith

  13. Mesoionic Compounds

    Indian Academy of Sciences (India)

    Organic Chemistry. Kamatak University,. Dharwad. Her research interests are synthesis, reactions and synthetic utility of sydnones. She is currently working on electrochemical and insecticidal/antifungal activities for some of these compounds. Keywords. Aromaticity, mesoionic hetero- cycles, sydnones, tandem re- actions.

  14. Analytical chemical system for the determination of heavy metals and organic compounds. Annual progress report, December 1, 1978-November 30, 1979

    Energy Technology Data Exchange (ETDEWEB)

    Siggia, S.; Barnes, R.M.

    1979-10-24

    Progress has been made in the synthesis and characterization of new resins for sequestering inorganic and organic compounds. The capabilities of the poly(dithiocarbamate) resin have been extended, a new poly(acrylamidoxime) resin prepared and characterized, and a series of resins for organic compounds prepared and tested. Limited actual sample analyses have been performed with these resins. A new inductively coupled plasma source, spectrometer, and computer system have been received and they are undergoing tests and installation. With this system in place, the multielement analysis of metals during the forthcoming period will insure the application of sequestering resins to practical analysis of energy-related materials. An automated sample handling and data system has been designed, some components purchased, and construction is scheduled for 1980.

  15. Analytical chemical system for the determination of heavy metals and organic compounds. Annual progress report, December 1, 1978-November 30, 1979

    International Nuclear Information System (INIS)

    Siggia, S.; Barnes, R.M.

    1979-01-01

    Progress has been made in the synthesis and characterization of new resins for sequestering inorganic and organic compounds. The capabilities of the poly(dithiocarbamate) resin have been extended, a new poly(acrylamidoxime) resin prepared and characterized, and a series of resins for organic compounds prepared and tested. Limited actual sample analyses have been performed with these resins. A new inductively coupled plasma source, spectrometer, and computer system have been received and they are undergoing tests and installation. With this system in place, the multielement analysis of metals during the forthcoming period will insure the application of sequestering resins to practical analysis of energy-related materials. An automated sample handling and data system has been designed, some components purchased, and construction is scheduled for 1980

  16. Liquid chromatography coupled to on-line post column derivatization for the determination of organic compounds: A review on instrumentation and chemistries

    International Nuclear Information System (INIS)

    Zacharis, Constantinos K.; Tzanavaras, Paraskevas D.

    2013-01-01

    Graphical abstract: -- Highlights: •Review on liquid chromatography coupled to post-column derivatization. •Overview of instrumentation for post-column derivatization. •Post-column chemistries for analysis of organic compounds. -- Abstract: Analytical derivatization either in pre or post column modes is one of the most widely used sample pretreatment techniques coupled to liquid chromatography. In the present review article we selected to discuss the post column derivatization mode for the analysis of organic compounds. The first part of the review focuses to the instrumentation of post-column setups including not only fundamental components such as pumps and reactors but also less common parts such as static mixers and back-pressure regulators; the second part of the article discusses the most popular “chemistries” that are involved in post column applications, including reagent-less approaches and new sensing platforms such as the popular gold nanoparticles. Some representative recent applications are also presented as tables

  17. Liquid chromatography coupled to on-line post column derivatization for the determination of organic compounds: A review on instrumentation and chemistries

    Energy Technology Data Exchange (ETDEWEB)

    Zacharis, Constantinos K., E-mail: zacharis@chem.auth.gr [Laboratory of Analytical Chemistry, Department of Chemistry, Aristotelian University of Thessaloniki, GR-54124 Thessaloniki (Greece); Department of Food Technology, School of Food Technology and Nutrition, Alexander Technological Educational Institute (ATEI) of Thessaloniki, 57400 Thessaloniki (Greece); Tzanavaras, Paraskevas D., E-mail: ptzanava@chem.auth.gr [Laboratory of Analytical Chemistry, Department of Chemistry, Aristotelian University of Thessaloniki, GR-54124 Thessaloniki (Greece)

    2013-10-10

    Graphical abstract: -- Highlights: •Review on liquid chromatography coupled to post-column derivatization. •Overview of instrumentation for post-column derivatization. •Post-column chemistries for analysis of organic compounds. -- Abstract: Analytical derivatization either in pre or post column modes is one of the most widely used sample pretreatment techniques coupled to liquid chromatography. In the present review article we selected to discuss the post column derivatization mode for the analysis of organic compounds. The first part of the review focuses to the instrumentation of post-column setups including not only fundamental components such as pumps and reactors but also less common parts such as static mixers and back-pressure regulators; the second part of the article discusses the most popular “chemistries” that are involved in post column applications, including reagent-less approaches and new sensing platforms such as the popular gold nanoparticles. Some representative recent applications are also presented as tables.

  18. Compounds enhanced in a mass spectrometric profile of smokers' exhaled breath versus non-smokers as determined in a pilot study using PTR-MS.

    Science.gov (United States)

    Kushch, Ievgeniia; Schwarz, Konrad; Schwentner, Lukas; Baumann, Bettina; Dzien, Alexander; Schmid, Alex; Unterkofler, Karl; Gastl, Günter; Spaněl, Patrik; Smith, David; Amann, Anton

    2008-06-01

    A pilot study has been carried out to define typical characteristics of the trace gas compounds in exhaled breath of non-smokers and smokers to assist interpretation of breath analysis data from patients who smoke with respiratory diseases and lung cancer. Exhaled breath was analyzed using proton transfer reaction-mass spectrometry (PTR-MS) for 370 volunteers (81 smokers, 210 non-smokers, 79 ex-smokers). Volatile organic compounds corresponding to product ions at seven mass-to-charge ratios (m/z 28, 42, 69, 79, 93, 97, 123) in the PTR-MS spectra differentiated between smokers and non-smokers. The Youden index (= maximum of sensitivity + specificity - 1, YI) as a measure for differentiation between smokers and non-smokers was YI = 0.43 for ions at the m/z values 28 (tentatively identified as HCN), YI = 0.75 for m/z = 42 (tentatively identified as acetonitrile) and YI = 0.53 for m/z = 79 (tentatively identified as benzene). No statistically significant difference between smokers and non-smokers was observed for the product ions at m/z = 31 and 33 (compounds tentatively identified as formaldehyde and methanol). When interpreting the exhaled breath of lung cancer or COPD patients, who often smoke, compounds appearing at the above-mentioned seven mass-to-charge ratios should be considered with appropriate care to avoid misdiagnosis. Validation studies in larger numbers of patients with more precise delineation of their smoking behavior and using additional analytical techniques such as GC/MS and SIFT-MS should be carried out.

  19. Using docking and alchemical free energy approach to determine the binding mechanism of eEF2K inhibitors and prioritizing the compound synthesis.

    Science.gov (United States)

    Wang, Qiantao; Edupuganti, Ramakrishna; Tavares, Clint D J; Dalby, Kevin N; Ren, Pengyu

    2015-01-01

    A-484954 is a known eEF2K inhibitor with submicromolar IC50 potency. However, the binding mechanism and the crystal structure of the kinase remains unknown. Here, we employ a homology eEF2K model, docking and alchemical free energy simulations to probe the binding mechanism of eEF2K, and in turn, guide the optimization of potential lead compounds. The inhibitor was docked into the ATP-binding site of a homology model first. Three different binding poses, hypothesis 1, 2, and 3, were obtained and subsequently applied to molecular dynamics (MD) based alchemical free energy simulations. The calculated relative binding free energy of the analogs of A-484954 using the binding pose of hypothesis 1 show a good correlation with the experimental IC50 values, yielding an r (2) coefficient of 0.96 after removing an outlier (compound 5). Calculations using another two poses show little correlation with experimental data, (r (2) of less than 0.5 with or without removing any outliers). Based on hypothesis 1, the calculated relative free energy suggests that bigger cyclic groups, at R1 e.g., cyclobutyl and cyclopentyl promote more favorable binding than smaller groups, such as cyclopropyl and hydrogen. Moreover, this study also demonstrates the ability of the alchemical free energy approach in combination with docking and homology modeling to prioritize compound synthesis. This can be an effective means of facilitating structure-based drug design when crystal structures are not available.

  20. Development of a Polyphenol Oxidase Biosensor from Jenipapo Fruit Extract (Genipa americana L. and Determination of Phenolic Compounds in Textile Industrial Effluents

    Directory of Open Access Journals (Sweden)

    Rafael Souza Antunes

    2018-05-01

    Full Text Available In this work, an innovative polyphenol oxidase biosensor was developed from Jenipapo (Genipa americana L. fruit and used to assess phenolic compounds in industrial effluent samples obtained from a textile industry located in Jaraguá-GO, Brasil. The biosensor was prepared and optimized according to: the proportion of crude vegetal extract, pH and overall voltammetric parameters for differential pulse voltammetry. The calibration curve presented a linear interval from 10 to 310 µM (r2 = 0.9982 and a limit of detection of 7 µM. Biosensor stability was evaluated throughout 15 days, and it exhibited 88.22% of the initial response. The amount of catechol standard recovered post analysis varied between 87.50% and 96.00%. Moreover, the biosensor was able to detect phenolic compounds in a real sample, and the results were in accordance with standard spectrophotometric assays. Therefore, the innovatively-designed biosensor hereby proposed is a promising tool for phenolic compound detection and quantification when environmental contaminants are concerned.

  1. Compound odontoma

    Directory of Open Access Journals (Sweden)

    Monica Yadav

    2012-01-01

    Full Text Available Odontomas have been extensively reported in the dental literature, and the term refers to tumors of odontogenic origin. Though the exact etiology is still unknown, the postulated causes include: local trauma, infection, inheritance and genetic mutation. The majority of the lesions are asymptomatic; however, may be accompanied with pain and swelling as secondary complaints in some cases. Here, we report a case of a compound odontome in a 14 year old patient.

  2. Experimental setup and analytical methods for the non-invasive determination of volatile organic compounds, formaldehyde and NOx in exhaled human breath

    International Nuclear Information System (INIS)

    Riess, Ulrich; Tegtbur, Uwe; Fauck, Christian; Fuhrmann, Frank; Markewitz, Doreen; Salthammer, Tunga

    2010-01-01

    Different analytical devices were tested and evaluated for their suitability of breath gas analysis by examining the physiological parameters and chemical substances in the exhaled breath of ten healthy probands during light cycling in dependence of methanol-rich nutrition. The probands exercised under normal breathing conditions on a bicycle ergometer. Breath air was exhaled into a glass cylinder and collected under steady-state conditions. Non-invasively measured parameters were pulse rate, breath frequency, temperature, relative humidity, NO x , total volatile organic compounds (TVOC PAS ), carbon dioxide (CO 2 ), formaldehyde, methanol, acetaldehyde, acetone, isoprene and volatile organic compounds (VOCs). Methanol rich food and beverages strongly influenced the concentration of methanol and other organic substances in human breath. On the other hand, nutrition and smoking had no clear effect on the physical conditions of the probands. The proton transfer reaction mass spectrometry (PTR-MS) method was found to be very suitable for the analysis of breath gas but the m/z 31, if assigned to formaldehyde, is sensitive to interferences. The time vs. concentration curves of nitric oxide showed sudden peaks up to 120 ppb in most of the measurements. In one case a strong interference of the NO x signal was observed. The time resolved analysis of exhaled breath gas is of high capability and significance for different applications if reliable analytical techniques are used. Some compounds like nitric oxide (NO), methanol, different VOCs as well as sum parameters like TVOC PAS are especially suitable as markers. Formaldehyde, which is rapidly metabolized in the human body, could be measured reliably as a trace component by the acetylacetone (acac) method but not by PTR-MS.

  3. Experimental setup and analytical methods for the non-invasive determination of volatile organic compounds, formaldehyde and NO{sub x} in exhaled human breath

    Energy Technology Data Exchange (ETDEWEB)

    Riess, Ulrich; Tegtbur, Uwe [Hannover Medical School, Sports Physiology and Sports Medicine, Carl-Neuberg-Str. 1, 30625 Hannover (Germany); Fauck, Christian; Fuhrmann, Frank; Markewitz, Doreen [Fraunhofer WKI, Department of Material Analysis and Indoor Chemistry, Bienroder Weg 54 E, 38108 Braunschweig (Germany); Salthammer, Tunga, E-mail: tunga.salthammer@wki.fraunhofer.de [Fraunhofer WKI, Department of Material Analysis and Indoor Chemistry, Bienroder Weg 54 E, 38108 Braunschweig (Germany)

    2010-06-11

    Different analytical devices were tested and evaluated for their suitability of breath gas analysis by examining the physiological parameters and chemical substances in the exhaled breath of ten healthy probands during light cycling in dependence of methanol-rich nutrition. The probands exercised under normal breathing conditions on a bicycle ergometer. Breath air was exhaled into a glass cylinder and collected under steady-state conditions. Non-invasively measured parameters were pulse rate, breath frequency, temperature, relative humidity, NO{sub x}, total volatile organic compounds (TVOC{sub PAS}), carbon dioxide (CO{sub 2}), formaldehyde, methanol, acetaldehyde, acetone, isoprene and volatile organic compounds (VOCs). Methanol rich food and beverages strongly influenced the concentration of methanol and other organic substances in human breath. On the other hand, nutrition and smoking had no clear effect on the physical conditions of the probands. The proton transfer reaction mass spectrometry (PTR-MS) method was found to be very suitable for the analysis of breath gas but the m/z 31, if assigned to formaldehyde, is sensitive to interferences. The time vs. concentration curves of nitric oxide showed sudden peaks up to 120 ppb in most of the measurements. In one case a strong interference of the NO{sub x} signal was observed. The time resolved analysis of exhaled breath gas is of high capability and significance for different applications if reliable analytical techniques are used. Some compounds like nitric oxide (NO), methanol, different VOCs as well as sum parameters like TVOC{sub PAS} are especially suitable as markers. Formaldehyde, which is rapidly metabolized in the human body, could be measured reliably as a trace component by the acetylacetone (acac) method but not by PTR-MS.

  4. Determination of the phenolic content and antioxidant potential of crude extracts and isolated compounds from leaves of Cordia multispicata and Tournefortia bicolor.

    Science.gov (United States)

    Correia Da Silva, Thiago B; Souza, Vivian Karoline T; Da Silva, Ana Paula F; Lyra Lemos, Rosangela P; Conserva, Lucia M

    2010-01-01

    In this work, the total phenolic content and antioxidant activity of extracts and four flavonoids isolated from leaves of two Boraginaceae species (Cordia multispicata Cham. and Tournefortia bicolor Sw.) were evaluated using Folin-Ciocalteu reagent, DPPH free radical scavenging and inhibition of peroxidation of linoleic acid by FTC method. For comparison, ascorbic acid, alpha-tocopherol and BHT were used. In general, extracts from T. bicolor (68.8 +/- 0.001 to > 1000 mg/g) showed higher phenolic content than C. multispicata (66.1 +/- 0.009 to 231 +/- 0.07 mg/g), and also scavenged radicals (IC(50) 12.8 +/- 2.5 to 437 +/- 3.5 mg/L) and inhibited lipid peroxide formation (IC(50) 51.2 +/- 2.29 to 89 +/- 0.59 mg/L). For these extracts a good correlation between the phenolic content and antioxidant activity was observed, suggesting that T. bicolor is richer in phenolic compounds and that it could serve as a new source of natural antioxidants or nutraceuticals with potential applications. Chromatographic procedures monitored by antioxidant assays afforded seven compounds, which were identified by spectral analyses (IR, MS and 1D and 2D NMR) and comparison with reported data as being trans-phytol (1), taraxerol (2), 3,7,4'-trimethoxyflavone (3), 5,3'-dihydroxy-3,7,4'-trimethoxyflavone (4), quercetin (5), tiliroside (6), and rutin (7). Compounds (4-7) were also evaluated and were effective as DPPH quenching (IC(50) 7.7 +/- 3.6 to 79.3 +/- 3.4 mg/L) and as inhibition of lipid peroxidation (IC(50) 80.1 +/- 0.98 to 88.7 +/- 3.62 mg/L). This is the first report on the total phenolic content, radical-scavenging and antioxidant activities of these species.

  5. Identification and quantification of estrogenic compounds in recycled and virgin paper for household use as determined by an in vitro yeast estrogen screen and chemical analysis

    DEFF Research Database (Denmark)

    Vinggaard, Anne; Körner, Wolfgang; Lund, Kirsten H.

    2000-01-01

    The use of recycled paper for the manufacture of food contact materials is widespread, but very little is known about the presence of potential contaminants in the paper. The purpose of this study was to assess the worst-case migration of estrogenic active compounds using extracts of paper...... contain bisphenol A and other xenoestrogens may apply to other types of recycled paper used for food packaging and emphasize the importance of identifying this and other contaminants in recycled paper in general. These data indicate that bisphenol A may be useful as a purity indicator for recycled paper....

  6. Determination of fatty acids and volatile compounds in fruits of rosehip(Rosa L.) species by HS-SPME/GC-MS and Im-SPME/GC-MS techniques

    OpenAIRE

    MURATHAN, ZEHRA TUĞBA; ZARIFIKHOSROSHAHI, MOZGAN; KAFKAS, NESİBE EBRU

    2016-01-01

    In this study, we aimed to compare fatty acid and volatile compound compositions of four rosehip species, namely Rosa pimpinellifolia, R. Villosa, R. Canina, and R. Dumalis, by gas chromatography with flame ionization detector (GC/FID) and headspace and immersion solid-phase microextraction gas chromatography-mass spectrometry (HS-SPME/GC-MS and Im-SPME/GC-MS) techniques. The total lipid contents in fruits of the rosehip species varied from 5.83% (R. Villosa) to 7.84% (R. Dumalis). A total of...

  7. Determination of high molecular mass compounds from Amazonian plant's leaves; Determinacao de compostos de massa molecular alta em folhas de plantas da Amazonia

    Energy Technology Data Exchange (ETDEWEB)

    Siqueira, Denilson Soares de; Pereira, Alberto dos Santos; Aquino Neto, Francisco Radler de [Universidade Federal, Rio de Janeiro, RJ (Brazil). Inst. de Quimica]. E-mail: ladetec@iq.gov.br; Cabral, Jose Augusto; Ferreira, Carlos Alberto Cid [Instituto Nacional de Pesquisas da Amazonia (INPA), Manaus, AM (Brazil); Simoneit, Bernd R.T. [Oregon State Univ., Corvallis, OR (United States). College of Oceanic and Atmospheric Sciences. Petroleum and Environmental Geochemistry Group; Elias, Vladimir O. [Analytical Solution, Rio de Janeiro, RJ (Brazil)

    2003-10-01

    The fractions of dichloromethane extracts of leaves from andiroba (Carapa guianensis - Meliaceae), caapi (Banisteriopsis caapi - Malpighiaceae), cocoa (Theobroma cacao - Sterculiaceae), Brazil nut (Bertholletia excelsa - Lecytidaceae), cupuacu (Theobroma grandiflorum - Sterculiaceae), marupa (Simaruba amara - Simaroubaceae) and rubber tree (Hevea brasiliensis - Euphorbiaceae), were analyzed by HT-HRGC and HT-HRGC-MS. Esters of homologous series of fatty acids and long chain alcohols, phytol, amyrines and tocopherols were characterized. The characterization of the compounds was based mainly in mass spectra data and in addition by usual spectrometric data ({sup 1}H and {sup 13}C NMR, IR). (author)

  8. Determination of polydimethylsiloxane–water partition coefficients for ten 1-chloro-4-[2,2,2-trichloro-1-(4-chlorophenyl)ethyl]benzene-related compounds and twelve polychlorinated biphenyls using gas chromatography/mass spectrometry

    Science.gov (United States)

    Eganhouse, Robert P.

    2016-01-01

    Polymer-water partition coefficients (Kpw) of ten DDT-related compounds were determined in pure water at 25 °C using commercial polydimethylsiloxane-coated optical fiber. Analyte concentrations were measured by thermal desorption-gas chromatography/full scan mass spectrometry (TD–GC/MSFS; fibers) and liquid injection-gas chromatography/selected ion monitoring mass spectrometry (LI–GC/MSSIM; water). Equilibrium was approached from two directions (fiber uptake and depletion) as a means of assessing data concordance. Measured compound-specific log Kpw values ranged from 4.8 to 6.1 with an average difference in log Kpw between the two approaches of 0.05 log units (∼12% of Kpw). Comparison of the experimentally-determined log Kpw values with previously published data confirmed the consistency of the results and the reliability of the method. A second experiment was conducted with the same ten DDT-related compounds and twelve selected PCB (polychlorinated biphenyl) congeners under conditions characteristic of a coastal marine field site (viz., seawater, 11 °C) that is currently under investigation for DDT and PCB contamination. Equilibration at lower temperature and higher ionic strength resulted in an increase in log Kpw for the DDT-related compounds of 0.28–0.49 log units (61–101% of Kpw), depending on the analyte. The increase in Kpw would have the effect of reducing by approximately half the calculated freely dissolved pore-water concentrations (Cfree). This demonstrates the importance of determining partition coefficients under conditions as they exist in the field.

  9. Spectro colorimetric and GC-MS Models, Used to Determine the Changes in the Natural Compounds of the Sea Buck thorn Leaves Sterilized with Ionizing Radiations

    International Nuclear Information System (INIS)

    Minea, R.; Popescu, M.I.; Sima, E.; Dumitrascu, M.; Culea, M.; Manea, St.; Mazilu, E.

    2009-01-01

    Spectro colorimetric and GC-MS methods were developed for the quantitative and quality analyze of the fatty acid methyl esters (FAME) and of some natural compounds extracted from the Sea Buckthorn (Hippophae rhamnoides) leaves sterilized by treating them with accelerated electron beams, generated by a linear accelerator. The spectro colorimetric models describe and easy controls the color as it relies on the psycho physics of the color perception and on the simple colorimetric models. Hunter Lab, CIELAB, CIELCH simple colorimetric models are used in developing complex colorimetric models and for the calculation of simple colorimetric models expressed as the total color difference between a sample and a witness, ΔΕ * , ΔΕ C MC, ΔΕ * D IN99, ΔΕ * C IE2000. They provide qualitative data on the deterioration of the active compounds by irradiation. If they are validated by GC-MS methods, they can also provide quantitative data on the radioinduced changes caused to the Sea Buckthorn leaves. The developed GC-MS methods allow the validation of the spectro colorimetric methods for the quantitative and qualitative evaluation of the radioinduced changes in the Sea Buckthorn leaves, reducing both the analyze times and the analyze cost, respectively the random errors of the procedures for extraction and derivation applied to samples preparation

  10. Improved in-tube electro-membrane extraction followed by high-performance liquid chromatography for simple and selective determination of ionic compounds: Optimization by central composite design.

    Science.gov (United States)

    Bazregar, Mohammad; Rajabi, Maryam; Yamini, Yadollah; Asghari, Alireza

    2017-07-01

    In this work, an efficient sample clean-up method, named in-tube electro-membrane extraction, is modified to resolve the formation of bubbles in the extraction process. This modified method is applied for the extraction of two model analytes including tartrazine and sunset yellow from food samples. The method is based on the electro-kinetic migration of ionized compounds by the application of an electrical potential difference, and on this basis the analytes under investigation, as anionic compounds, simply migrate from the donor phase and concentrate in the acceptor phase. A thin polypropylene sheet placed in the tube acts as a support for the membrane solvent, and it separates 30 μL of the aqueous acceptor from 1.2 mL of the aqueous donor. This setup can be used to solve the problem of extracting highly hydrophilic analytes. Response surface methodology is used for optimization of the experimental parameters so that under the optimized conditions, the method provides a good linearity in the range of 50-1000 ng/mL, low limits of detection (15-25 ng/mL), good extraction repeatabilities (relative standard deviations below 8.1%, n = 5), and high extraction recoveries (54-76%). © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Determination and Identification of a Specific Marker Compound for Discriminating Shrub Chaste Tree Fruit from Agnus Castus Fruit Based on LC/MS Metabolic Analysis.

    Science.gov (United States)

    Yahagi, Tadahiro; Masada, Sayaka; Oshima, Naohiro; Suzuki, Ryuta; Matsufuji, Hiroshi; Takahashi, Yutaka; Watanabe, Masato; Yahara, Shoji; Iida, Osamu; Kawahara, Nobuo; Maruyama, Takuro; Goda, Yukihiro; Hakamatsuka, Takashi

    2016-01-01

    Shrub Chaste Tree Fruit (SCTF) is defined as the fruits of Vitex rotundifolia L. f. and V. trifolia L. and has been used as a component of some traditional Japanese medicines (Kampo formulations). Agnus Castus Fruit (ACF) is defined as the dried ripe fruits of V. agnus-castus L.; it is used in traditional European medicines, but is becoming popular in Japan as both an over-the-counter drug and as an ingredient in health foods for treating premenstrual syndrome (PMS). To ensure the efficacy and safety of both SCTF and ACF products, it is important to precisely authenticate their botanical origins and to clearly distinguish between SCTF and ACF. Therefore, we tried to identify SCTF-specific marker compounds based on LC/MS metabolic analysis. The multivariate analysis of LC/MS data from SCTF and ACF samples furnished candidate marker compounds of SCTF. An SCTF-specific marker was isolated from SCTF crude drugs and identified as 3-O-trans-feruloyl tormentic acid on the basis of spectroscopic data from NMR and MS. Since avoiding contamination from closely related species is a significant requirement for pharmaceuticals of natural origin, this information will be valuable for the quality control of both SCTF and ACF products from the viewpoint of regulatory science.

  12. Simultaneous Determination of Perfluorinated Compounds in Edible Oil by Gel-Permeation Chromatography Combined with Dispersive Solid-Phase Extraction and Liquid Chromatography-Tandem Mass Spectrometry.

    Science.gov (United States)

    Yang, Lili; Jin, Fen; Zhang, Peng; Zhang, Yanxin; Wang, Jian; Shao, Hua; Jin, Maojun; Wang, Shanshan; Zheng, Lufei; Wang, Jing

    2015-09-30

    A simple analytical method was developed for the simultaneous analysis of 18 perfluorinated compounds (PFCs) in edible oil. The target compounds were extracted by acetonitrile, purified by gel permeation chromatography (GPC) and dispersive solid-phase extraction (DSPE) using graphitized carbon black (GCB) and octadecyl (C18), and analyzed by liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ES-MS/MS) in negative ion mode. Recovery studies were performed at three fortification levels. The average recoveries of all target PFCs ranged from 60 to 129%, with an acceptable relative standard deviation (RSD) (1-20%, n = 3). The method detection limits (MDLs) ranged from 0.004 to 0.4 μg/kg, which was significantly improved compared with the existing liquid-liquid extraction and cleanup method. The method was successfully applied for the analysis of all target PFCs in edible oil samples collected from markets in Beijing, China, and the results revealed that C6-C10 perfluorocarboxylic acid (PFCAs) and C7 perfluorosulfonic acid PFSAs were the major PFCs detected in oil samples.

  13. [Simultaneous determination of four compounds in Sanjing Shuanghuanglian Oral Liquid by high performance liquid chromatography-diode array detection-electrochemical detection].

    Science.gov (United States)

    Liu, Lin; Suo, Zhirong; Zheng, Jianbin

    2006-05-01

    Chlorogenic acid, caffeic acid, baicalin and luteolin in Sanjing Shuanghuanglian Oral Liquid were simultaneously detected and identified using a high performance liquid chromatography coupled with diode array detection and electrochemical detection (HPLC-DAD-ECD). The separation was performed on a Zorbax SB-C18 column (150 mm x 4.6 mm i. d., 5.0 microm). The mobile phase consisted of (A) methanol and (B) methanol-water-acetic acid (50: 50: 1, v/v/v) using a linear gradient elution of 2%A-3%A at 0-3 min, 3%A-25%A at 3-15 min, 25%A-80%A at 15-20 min. The flow rate was 0.8 mL/min. The DAD detection was used at 275 nm. The ECD detection was done at 0.7 V. The column thermostat set at 30 degrees C. The limits of detection of the 4 compounds were 1 mg/L for chlorogenic acid, 0.2 mg/L for caffeic acid, 9 mg/L for baicalin, 7 mg/L for luteolin. The average recoveries were between 96.6%-99.6% with relative standard deviations (RSDs) of 2.5%-4.1%. The method is simple, rapid, reproducible and accurate. It can be used for the routine analysis of the four compounds in Shuanghuanglian Oral Liquid.

  14. World-wide and regional intercomparison for the determination of organochlorine compounds and petroleum hydrocarbons in sediment sample IAEA-357. Report no. 51

    International Nuclear Information System (INIS)

    Villeneuve, J.P.; Mee, L.D.

    1992-06-01

    This report describes the results of IAEA/UNEP intercomparison run 357 for the chemical analysis of organochlorine compounds and petroleum hydrocarbons in marine sediments. The Marine Environmental Studies Laboratory (MESL) of IAEA-MEL has conducted intercomparison exercises on trace organic compounds for over ten years as part of its contribution to IAEA's analytical quality control service and UNEP's regional seas programme and occasionally in association with the intergovernmental oceanographic Commission (of UNESCO) GIPME programme. Results of previous exercises have revealed serious problems for many regional laboratories to obtain comparable data. This, in turn, has raised serious concerns on the validity of region-wide or global marine pollution assessments. Even more worrisome was the apparent lack of improvement in data quality from exercise to exercise. As a consequence of the above situation, it was decided to seek increased support for quality assurance programmes. Staff of MESL, with funding from UNEP, the World bank and regional trust funds, embarked on a campaign to train analysts in modern measurement techniques, supply appropriate and reliable reference methods and materials and, where possible, to improve analytical instruments in member states laboratories. This work continues at present and recent training programmes have been conducted in the Wider Caribbean, East Africa, The Gulf and the Mediterranean

  15. Simultaneous determination of five major compounds in the traditional medicine Pyeongwee-San by high performance liquid chromatography-diode array detection and liquid chromatography-mass spectrometry/mass spectrometry.

    Science.gov (United States)

    Lee, Bohyoung; Weon, Jin Bae; Yun, Bo-Ra; Lee, Jiwoo; Eom, Min Rye; Ma, Choong Je

    2014-01-01

    Pyeongwee-San (PWS) has been widely used for treating acute gastritis, chronic, and gastritis. In this paper, simultaneous determination of five compounds (naringin, hesperidin, glycyrrhizin, atractylenolide III, and magnolol) from traditional medicine PWS using the high performance liquid chromatography (HPLC) was established for quality control. Optimum separations were obtained with a SHISEIDO C18 reverse-phase column by gradient elution with 0.1% Trifluoroacetic acid (TFA) water-acetonitrile as the mobile phase. The flow rate was 1 mL/min and detection wavelength was set at 205 nm and 250 nm. Validation of the analytical method was evaluated by linearity, precision, and accuracy test. The calibration curves were linear over the established range with R (2) > 0.9978. The limit of detection (LOD) and limit of quantification (LOQ) ranged from 0.09 to 0.43 and 0.27 to 1.29 μg/mL. The method exhibited intra-day and inter-day precision range between 0.01-1.86% and 0.04-0.35% respectively. The recoveries of five compounds in PWS were in the range between 93.18-106.40%, and 0.20-1.51%. The application of this method was identified through the successful analysis of five compounds in 12 batches of PWS. In addition, identification of five compounds was confirmed by a liquid chromatography method and mass spectrometry. The HPLC method was could be accomplished to the quality control and stable experiment for the preparations consisted of five major compounds.

  16. Synthesis, crystal structure determination, thermal and magnetic properties of the new Cu{sub 0.73}Ni{sub 0.27}(HSeO{sub 3}){sub 2} compound

    Energy Technology Data Exchange (ETDEWEB)

    Hentech, I., E-mail: hentechimen@yahoo.fr [Laboratoire des Sciences des Matériaux et de l' Environnement, Faculté des Sciences de Sfax, BP 1171, Université de Sfax, 3000 (Tunisia); CMTR, ICMPE, UMR7182, CNRS – Université Paris Est Créteil, 2-8 rue Henri Dunant, F-94320 Thiais (France); Zehani, K. [CMTR, ICMPE, UMR7182, CNRS – Université Paris Est Créteil, 2-8 rue Henri Dunant, F-94320 Thiais (France); Kabadou, A.; Ben Salah, A.; Loukil, M. [Laboratoire des Sciences des Matériaux et de l' Environnement, Faculté des Sciences de Sfax, BP 1171, Université de Sfax, 3000 (Tunisia); Bessais, L. [CMTR, ICMPE, UMR7182, CNRS – Université Paris Est Créteil, 2-8 rue Henri Dunant, F-94320 Thiais (France)

    2017-01-15

    A novel three-dimensional Cu{sub 0.73}Ni{sub 0.27}(HSeO{sub 3}){sub 2} compound was prepared from an aqueous solution. This compound crystallizes in the monoclinic system with P2{sub 1}/n space group and with the following cell parameters: a=6.4379(3) Å; b=7.3555(3) Å; c=5.7522(3) Å; β=93.4341(1)°; V=271.90(2) Å{sup 3} and Z=2. The reported material has been structurally characterized by X-ray powder diffraction and confirmed by scanning electron microscope and energy dispersive spectroscopy (MEB/EDS) analysis. The copper/nickel atom is surrounded by an octahedron coordination of oxygen atoms from sex hydrogenoselenites anions. The presence of (HSeO{sub 3}){sup −} has been further confirmed by IR spectroscopy and this compound exhibits a phase transition at 356 K, this transition has been detected by differential scanning calorimetry and TG-DTA measurement. The magnetic property of this material was determined. The ferromagnetic ordering is further confirmed by the magnetic field dependence of the magnetization (Hysteresis loop) at 10 K. The substitution of Cu by Ni induces a ferro-paramagnetic transition at T=31 K. Field cooled (FC) and Zero field cooled (ZFC) magnetization measurements under an applied field of 100 Oe in the temperature range of 10–300 K were performed. These measurements have been resulted the blocking temperature (T{sub B}) at around 25 K. - Highlights: • A novel three-dimensional Cu{sub 0.73}Ni{sub 0.27}(HSeO{sub 3}){sub 2} compound was prepared from an aqueous solution. • Magnetic measurements reveal the occurrence of weak ferromagnetism at low temperature for this compound. • The substitution of Cu by Ni induces a ferro-paramagnetic transition at T=31 K.

  17. Magnesium compounds

    Science.gov (United States)

    Kramer, D.A.

    2007-01-01

    Seawater and natural brines accounted for about 52 percent of U.S. magnesium compounds production in 2006. Dead-burned magnesia was produced by Martin Marietta Magnesia Specialties from well brines in Michigan. Caustic-calcined magnesia was recovered from sea-water by Premier Chemicals in Florida; from well brines in Michigan by Martin Marietta and Rohm and Haas; and from magnesite in Nevada by Premier Chemicals. Intrepid Potash-Wendover and Great Salt Lake Minerals recovered magnesium chloride brines from the Great Salt Lake in Utah. Magnesium hydroxide was produced from brucite by Applied Chemical Magnesias in Texas, from seawater by SPI Pharma in Delaware and Premier Chemicals in Florida, and by Martin Marietta and Rohm and Haas from their operations mentioned above. About 59 percent of the magnesium compounds consumed in the United States was used for refractories that are used mainly to line steelmaking furnaces. The remaining 41 percent was consumed in agricultural, chemical, construction, environmental and industrial applications.

  18. Rapid Determination of Major Compounds in the Ethanol Extract of Geopropolis from Malaysian Stingless Bees, Heterotrigona itama, by UHPLC-Q-TOF/MS and NMR.

    Science.gov (United States)

    Zhao, Lingling; Yu, Mengjiao; Sun, Minghui; Xue, Xiaofeng; Wang, Tongtong; Cao, Wei; Sun, Liping

    2017-11-10

    A reliable, rapid analytical method was established for the characterization of constituents of the ethanol extract of geopropolis (EEGP) produced by Malaysian stingless bees- Heterotrigona itama -by combining ultra-high-performance liquid chromatography with quadruple time-of-flight mass spectrometry (UHPLC-Q-TOF/MS). Based on known standards, the online METLIN database, and published literature, 28 compounds were confirmed. Phenolic acids, flavones, triterpenes and phytosterol were identified or tentatively identified using characteristic diagnostic fragment ions. The results indicated that terpenoids were the main components of EEGP, accompanied by low levels of phenolic acids, flavonoids, and phytosterol. Two major components were further purified by preparative high-performance liquid chromatography (PHPLC) and identified by nuclear magnetic resonance (NMR) as 24( E )-cycloart-24-ene-26-ol-3-one and 20-hydroxy-24-dammaren-3-one. These two triterpenes, confirmed in this geopropolis for the first time, are potential chemical markers for the identification of geopropolis from Malaysian stingless bees, H. itama .

  19. Implementing DBS methodology for the determination of Compound A in monkey blood: GLP method validation and investigation of the impact of blood spreading on performance.

    Science.gov (United States)

    Fan, Leimin; Lee, Jacob; Hall, Jeffrey; Tolentino, Edward J; Wu, Huaiqin; El-Shourbagy, Tawakol

    2011-06-01

    This article describes validation work for analysis of an Abbott investigational drug (Compound A) in monkey whole blood with dried blood spots (DBS). The impact of DBS spotting volume on analyte concentration was investigated. The quantitation range was between 30.5 and 10,200 ng/ml. Accuracy and precision of quality controls, linearity of calibration curves, matrix effect, selectivity, dilution, recovery and multiple stabilities were evaluated in the validation, and all demonstrated acceptable results. Incurred sample reanalysis was performed with 57 out of 58 samples having a percentage difference (versus the mean value) less than 20%. A linear relationship between the spotting volume and the spot area was drawn. The influence of spotting volume on concentration was discussed. All validation results met good laboratory practice acceptance requirements. Radial spreading of blood on DBS cards can be a factor in DBS concentrations at smaller spotting volumes.

  20. Determination of Volatile Organic Compounds (VOCs from Wrapping Films and Wrapped PDO Italian Cheeses by Using HS-SPME and GC/MS

    Directory of Open Access Journals (Sweden)

    Sara Panseri

    2014-06-01

    Full Text Available Nowadays food wrapping assures attractive presentation and simplifies self-service shopping. Polyvinylchloride (PVC- and polyethylene (PE-based cling-films are widely used worldwide for wrapping cheeses. For this purpose, films used in retail possess suitable technical properties such as clinginess and unrolling capacity, that are achieved by using specific plasticizers during their manufacturing process. In the present study, the main VOCs of three cling-films (either PVC-based or PE-based for retail use were characterized by means of Solid-Phase Micro-Extraction and GC/MS. In addition, the effects of cling film type and contact time on the migration of VOCs from the films to four different PDO Italian cheeses during cold storage under light or dark were also investigated. Among the VOCs isolated from cling-films, PVC released 2-ethylhexanol and triacetin. These compounds can likely be considered as a “non-intentionally added substance”. These same compounds were also detected in cheeses wrapped in PVC films with the highest concentration found after 20 days storage. The PE cling-film was shown to possess a simpler VOC profile, lacking some molecules peculiar to PVC films. The same conclusions can be drawn for cheeses wrapped in the PE cling-film. Other VOCs found in wrapped cheeses were likely to have been released either by direct transfer from the materials used for the manufacture of cling-films or from contamination of the films. Overall, HS-SPME is shown to be a rapid and solvent free technique to screen the VOCs profile of cling-films, and to detect VOCs migration from cling-films to cheese under real retail storage conditions.

  1. Microsomal cytochrome P450-3A4 (CYP3A4) nanobiosensor for the determination of 2,4-dichlorophenol-An endocrine disruptor compound

    Energy Technology Data Exchange (ETDEWEB)

    Hendricks, Nicolette R.; Waryo, Tesfaye T.; Arotiba, Omotayo; Jahed, Nazeem; Baker, Priscilla G.L. [SensorLab, Department of Chemistry, University of Western Cape, Moderddam Road, Bellville, Cape Town 7535 (South Africa); Iwuoha, Emmanuel I. [SensorLab, Department of Chemistry, University of Western Cape, Moderddam Road, Bellville, Cape Town 7535 (South Africa)], E-mail: eiwuoha@uwc.ac.za

    2009-02-28

    Cytochrome P450-3A4 (CYP3A4) is a monooxygenase enzyme that plays a major role in the detoxification of bioactive compounds and hydrophobic xenobiotics (e.g. medicines, drugs, environmental pollutants, food supplements and steroids). Physiologically the monooxygenation reactions of this class II, microsomal, b-type heme enzyme, usually requires cytochrome P450 reductase, NADPH. A novel CYP3A4 biosensor system that essentially simplified the enzymatic redox processes by allowing electron transfer between the electrode and the enzyme redox centre to occur, without any need for the physiological redox partners, was developed for the detection of 2,4-dichlorophenol (2,4-DCP), a priority environmental pollutant and an endocrine disruptor. The biosensor, GC/Naf-Co(Sep){sup 3+}/CYP3A4/Naf, was constructed by encapsulating CYP3A4 in a Nafion-cobalt (III) sepulchrate (Naf-Co(Sep){sup 3+}) composite film on a glassy carbon (GC) electrode. The responses of the biosensor to 2,4-dichlorophenol, erythromycin (CYP3A4 native substrate) and ketoconazole (CYP 3A4 natural inhibitor) were studied by cyclic and square wave voltammetric techniques. The detection limit (DL) of the biosensor for 2,4-dichlorophenol was 0.043 {mu}g L{sup -1}, which is by an order of magnitude lower than the EU limit (0.3 {mu}g L{sup -1}) for any pesticide compound in ground water. The biosensor's DL is lower than the U.S. Environmental Protection Agency's drinking water equivalent level (DWEL) value for 2,4-DCP, which is 2 {mu}g L{sup -1}.

  2. Microsomal cytochrome P450-3A4 (CYP3A4) nanobiosensor for the determination of 2,4-dichlorophenol-An endocrine disruptor compound

    International Nuclear Information System (INIS)

    Hendricks, Nicolette R.; Waryo, Tesfaye T.; Arotiba, Omotayo; Jahed, Nazeem; Baker, Priscilla G.L.; Iwuoha, Emmanuel I.

    2009-01-01

    Cytochrome P450-3A4 (CYP3A4) is a monooxygenase enzyme that plays a major role in the detoxification of bioactive compounds and hydrophobic xenobiotics (e.g. medicines, drugs, environmental pollutants, food supplements and steroids). Physiologically the monooxygenation reactions of this class II, microsomal, b-type heme enzyme, usually requires cytochrome P450 reductase, NADPH. A novel CYP3A4 biosensor system that essentially simplified the enzymatic redox processes by allowing electron transfer between the electrode and the enzyme redox centre to occur, without any need for the physiological redox partners, was developed for the detection of 2,4-dichlorophenol (2,4-DCP), a priority environmental pollutant and an endocrine disruptor. The biosensor, GC/Naf-Co(Sep) 3+ /CYP3A4/Naf, was constructed by encapsulating CYP3A4 in a Nafion-cobalt (III) sepulchrate (Naf-Co(Sep) 3+ ) composite film on a glassy carbon (GC) electrode. The responses of the biosensor to 2,4-dichlorophenol, erythromycin (CYP3A4 native substrate) and ketoconazole (CYP 3A4 natural inhibitor) were studied by cyclic and square wave voltammetric techniques. The detection limit (DL) of the biosensor for 2,4-dichlorophenol was 0.043 μg L -1 , which is by an order of magnitude lower than the EU limit (0.3 μg L -1 ) for any pesticide compound in ground water. The biosensor's DL is lower than the U.S. Environmental Protection Agency's drinking water equivalent level (DWEL) value for 2,4-DCP, which is 2 μg L -1

  3. Radioactive decay and labeled compounds

    International Nuclear Information System (INIS)

    Anon.

    1991-01-01

    This chapter on radioactive decay and labeled compounds has numerous intext equations and worked, sample problems. Topics covered include the following: terms and mathematics of radioactive decay; examples of calculations; graphs of decay equations; radioactivity or activity; activity measurements; activity decay; half-life determinations; labeled compounds. A 20 problem set is also included. 1 ref., 4 figs., 1 tab

  4. Compound odontoma

    Directory of Open Access Journals (Sweden)

    José Marcelo Vargas Pinto

    2008-01-01

    Full Text Available Odontomas are the most common types of odontogenic tumors, as they are considered more as a developmental anomaly (hamartoma than as a true neoplasia. The aim of the present study is to describe a clinical case of compound odontoma, analyzing its most commonsigns, its region of location, the decade of life and patient’s gender, disorders that may occur as well as the treatment proposed. In order to attain this objective, the method was description of the present clinical case and bibliographic revision, arriving at the result that the treatment for this type of lesion invariably is surgical removal (enucleation and curettage and the prognosis is excellent. The surgical result was followed up in the post-operative period by radiographic exam, and it was possible to conclude that there was complete cicatrization and tissue repair.

  5. Magnesium compounds

    Science.gov (United States)

    Kramer, D.A.

    2012-01-01

    Seawater and natural brines accounted for about 57 percent of magnesium compounds produced in the United States in 2011. Dead-burned magnesia was produced by Martin Marietta Magnesia Specialties LLC from well brines in Michigan. Caustic-calcined magnesia was recovered from seawater by Premier Magnesia LLC in Florida, from well brines in Michigan by Martin Marietta and from magnesite in Nevada by Premier Magnesia. Intrepid Potash Wendover LLC and Great Salt Lake Minerals Corp. recovered magnesium chloride brines from the Great Salt Lake in Utah. Magnesium hydroxide was produced from seawater by SPI Pharma Inc. in Delaware and Premier Magnesia in Florida, and by Martin Marietta from its brine operation in Michigan.

  6. The determination of solubility and diffusion coefficient for solids in liquids by an inverse measurement technique using cylinders of amorphous glucose as a model compound

    International Nuclear Information System (INIS)

    Hu, Chengyao; Huang, Pei

    2011-01-01

    The importance of sugar and sugar-containing materials is well recognized nowadays, owing to their application in industrial processes, particularly in the food, pharmaceutical and cosmetic industries. Because of the large numbers of those compounds involved and the relatively small number of solubility and/or diffusion coefficient data for each compound available, it is highly desirable to measure the solubility and/or diffusion coefficient as efficiently as possible and to be able to improve the accuracy of the methods used. In this work, a new technique was developed for the measurement of the diffusion coefficient of a stationary solid solute in a stagnant solvent which simultaneously measures solubility based on an inverse measurement problem algorithm with the real-time dissolved amount profile as a function of time. This study differs from established techniques in both the experimental method and the data analysis. The experimental method was developed in which the dissolved amount of solid solute in quiescent solvent was investigated using a continuous weighing technique. In the data analysis, the hybrid genetic algorithm is used to minimize an objective function containing a calculated and a measured dissolved amount with time. This is measured on a cylindrical sample of amorphous glucose in methanol or ethanol. The calculated dissolved amount, that is a function of the unknown physical properties of the solid solute in the solvent, is calculated by the solution of the two-dimensional nonlinear inverse natural convection problem. The estimated values of the solubility of amorphous glucose in methanol and ethanol at 293 K were respectively 32.1 g/100 g methanol and 1.48 g/100 g ethanol, in agreement with the literature values, and support the validity of the simultaneously measured diffusion coefficient. These results show the efficiency and the stability of the developed technique to simultaneously estimate the solubility and diffusion coefficient. Also

  7. X-ray magnetic circular dichroism in d and f ferromagnetic materials: recent theoretical progress. Part II

    International Nuclear Information System (INIS)

    Antonov, V.N.; Shpak, A.P.; Yares'ko, A.N.

    2008-01-01

    The present state of theoretical understanding of the x-ray magnetic circular dichroism (XMCD) of 4f and 5f compounds is reviewed. Energy band theory based upon the local spin-density approximation (LSDA) describes the XMCD spectra of transition metal compounds with high accuracy. However, the LSDA does not suffice for lanthanide compounds which have a correlated 4f shell. A satisfactory description of the XMCD spectra could be obtained by using a generalization of the LSDA, in which explicitly f electron Coulomb correlations are taken into account (LSDA+U approach). As examples of this group we consider the compound GdN. We also consider uranium 5f compounds. In those compounds where the 5f electrons are rather delocalized, the LSDA describes the XMCD spectra reasonably well. As an example of this group we consider UFe 2 . Particular differences occur for uranium compounds in which the 5f electrons are neither delocalized nor localized, but more or less semilocalized. Typical examples are UXAl (X=Co, Rh, and Pt), and UX (X=S, Se, Te). However, the semilocalized 5f's are not inert, but their interaction with conduction electrons plays an important role. We also consider the electronic structure and XMCD spectra of the heavy-fermion compounds UPt 3 , URu 2 Si 2 , UPd 2 Al 3 , UNi 2 Al 3 , and UBe 13 , where the degree of the 5f localization is increased in comparison with other uranium compounds. The electronic structure and XMCD spectra of UGe 2 which possesses simultaneously ferromagnetism and superconductivity also presented. Recently achieved improvements for describing 5f compounds are discussed

  8. Rapid Determination of Major Compounds in the Ethanol Extract of Geopropolis from Malaysian Stingless Bees, Heterotrigona itama, by UHPLC-Q-TOF/MS and NMR

    Directory of Open Access Journals (Sweden)

    Lingling Zhao

    2017-11-01

    Full Text Available A reliable, rapid analytical method was established for the characterization of constituents of the ethanol extract of geopropolis (EEGP produced by Malaysian stingless bees—Heterotrigona itama—by combining ultra-high-performance liquid chromatography with quadruple time-of-flight mass spectrometry (UHPLC-Q-TOF/MS. Based on known standards, the online METLIN database, and published literature, 28 compounds were confirmed. Phenolic acids, flavones, triterpenes and phytosterol were identified or tentatively identified using characteristic diagnostic fragment ions. The results indicated that terpenoids were the main components of EEGP, accompanied by low levels of phenolic acids, flavonoids, and phytosterol. Two major components were further purified by preparative high-performance liquid chromatography (PHPLC and identified by nuclear magnetic resonance (NMR as 24(E-cycloart-24-ene-26-ol-3-one and 20-hydroxy-24-dammaren-3-one. These two triterpenes, confirmed in this geopropolis for the first time, are potential chemical markers for the identification of geopropolis from Malaysian stingless bees, H. itama.

  9. Chemical analysis of phenolic compounds and determination of anti-oxidant, antimicrobial and cytotoxic activities of organic extracts of Pinus coulteri

    Directory of Open Access Journals (Sweden)

    Soumia Merah

    2018-05-01

    Full Text Available New bioactive natural products, the phenolic composition and the biological activities of organic extracts from the needles of the Algerian Pinus coulteri were investigated. The analysis by HPLC-DAD of crude extract revealed the presence of 10 phenolic acids and nine flavonoids. In vitro anti-oxidant activities were performed using four different tests. The greatest antiradical activity was found in the ethyl acetate fraction (IC50 = 3.2 ± 0.3 µg/mL, whereas the diethyl ether fraction had the higher contents of total phenolics and flavonoids and exhibited a highest activity in reducing power and β-carotene–linoleic acid tests with EC50= 67.1 ± 0.4 μg/mL and 71.5 ± 0.2% of inhibition, respectively. Furthermore, a low to moderate antimicrobial activity according to all extracts was revealed against eight bacteria tested. The MIC value of chloroform fraction showed a strong degree of antibacterial activity (<0.09 mg/mL. The crude extract was found toxic with LC50 value of 15.2 μg/mL by brine shrimp toxicity assay. The needle extract of P. coulteri is rich in valuable biologically active compounds and could represent a new resource of anti-oxidant agents for the treatment of diseases.

  10. Determination of the equilibrium miscibility gap in the Pd-Rh alloy system using metal nanopowders obtained by decomposition of coordination compounds

    Energy Technology Data Exchange (ETDEWEB)

    Shubin, Yu.V., E-mail: shubin@niic.nsc.ru; Plyusnin, P.E.; Korenev, S.V.

    2015-02-15

    Highlights: • The Pd-Rh phase diagram has been experimentally reinvestigated. • The true equilibrium was achieved with the two-way approach. • The critical point of the miscibility gap lie at 58 at.% Rh and 820 °C. - Abstract: The Pd-Rh phase diagram has been reinvestigated in the subsolidus region using X-ray diffraction, scanning and transmission electron microscopy. The true equilibrium at the miscibility boundary was achieved with the two-way approach. Nanosized powders of metastable solid solutions and two-phase palladium-rhodium mixtures were used to shorten the time required to equilibrate the system. The initial samples were prepared by decomposition of coordination compounds [Pd(NH{sub 3}){sub 2}Cl{sub 2}], [Rh(NH{sub 3}){sub 5}Cl]Cl{sub 2}, [Pd(NH{sub 3}){sub 4}]{sub 3}[Rh(NO{sub 2}){sub 6}]{sub 2} and [Pd(NH{sub 3}){sub 4}][Rh(NH{sub 3})(NO{sub 2}){sub 5}]. The obtained phase diagram exhibits miscibility gap wider than generally accepted with the critical point of solubility at 58 at.% Rh and 820 °C.

  11. Determination of descriptors for polycyclic aromatic hydrocarbons and related compounds by chromatographic methods and liquid-liquid partition in totally organic biphasic systems.

    Science.gov (United States)

    Ariyasena, Thiloka C; Poole, Colin F

    2014-09-26

    Retention factors on several columns and at various temperatures using gas chromatography and from reversed-phase liquid chromatography on a SunFire C18 column with various mobile phase compositions containing acetonitrile, methanol and tetrahydrofuran as strength adjusting solvents are combined with liquid-liquid partition coefficients in totally organic biphasic systems to calculate descriptors for 23 polycyclic aromatic hydrocarbons and eighteen related compounds of environmental interest. The use of a consistent protocol for the above measurements provides descriptors that are more self consistent for the estimation of physicochemical properties (octanol-water, air-octanol, air-water, aqueous solubility, and subcooled liquid vapor pressure). The descriptor in this report tend to have smaller values for the L and E descriptors and random differences in the B and S descriptors compared with literature sources. A simple atom fragment constant model is proposed for the estimation of descriptors from structure for polycyclic aromatic hydrocarbons. The new descriptors show no bias in the prediction of the air-water partition coefficient for polycyclic aromatic hydrocarbons unlike the literature values. Copyright © 2014 Elsevier B.V. All rights reserved.

  12. Use of a cranium-vessel determined by means of compound analysis; Uso de una vasija-craneo determinada por medio de analisis de compuesto

    Energy Technology Data Exchange (ETDEWEB)

    Leboreiro, I.; Pijoan, C.M.; Mansilla, J. [Direccion de Antropologia Fisica, INAH, Gandhi s/n, Polanco, 11560 Mexico D. F. (Mexico); Bosch, P. [Instituto de Investigaciones en Materiales, UNAM, Circuito Exterior, Ciudad Universitaria, 04510 Mexico D. F. (Mexico)

    2004-07-01

    Many human remains as bones, skin, teeth and others, were used in pre-hispanic cultures as tools or ritual objects. A human cranial vault filed in the Direccion de Antropologia Fisica presented particular and interesting cultural modifications. There are twelve drills used to restore by sewing the crane, in this way the piece resembles a pot. It has been established that it comes from North Mexico where such restoration work has been reported (Aveleyra, 1956) for containers made of vegetables (guaje). As the utilization of this kind of archaeological remain is unknown, the study of dust samples from the inside and the outside of the crane should provide hints on the products stored into it. In this study we present the X-ray diffraction results which show that the outer dusts are mainly constituted by albite, andesite and quartz, whereas in the inside the substances were mainly aluminosilicates and magnesium compounds. Hence, most probably, this crane was not used as a conventional container and it is linked to the concoction of magnesium and aluminosilicates containing products. This conclusion has to be correlated to that even nowadays, in both alternative and conventional medicine. (Author) 7 refs., 7 figs.

  13. Validated method for the determination of perfluorinated compounds in placental tissue samples based on a simple extraction procedure followed by ultra-high performance liquid chromatography-tandem mass spectrometry analysis.

    Science.gov (United States)

    Martín, J; Rodríguez-Gómez, R; Zafra-Gómez, A; Alonso, E; Vílchez, J L; Navalón, A

    2016-04-01

    Xenobiotic exposure during pregnancy is inevitable. Determination of perfluorinated compounds (PFCs), chemicals described as environmental contaminants by Public Health Authorities due to their persistence, bioaccumulation and toxicity, is a challenge. In the present work, a method based on a simplified sample treatment involving freeze-drying, solvent extraction and dispersive clean-up of the extracts using C18 sorbents followed by an ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) analysis was developed and validated for the determination of five perfluorinated carboxylic acids (C4-C8) and perfluorooctane sulfonate (PFOS) in placental tissue samples. The most influential parameters affecting the extraction method and clean-up were optimized using Design of Experiments (DOE). The method was validated using matrix-matched calibration. Found limits of detection (LODs) ranged from 0.03 to 2 ng g(-1) and limits of quantification (LOQs) from 0.08 to 6 ng g(-1), while inter- and intra-day variability was under 14% in all cases. Recovery rates for spiked samples ranged from 94% to 113%. The method was satisfactorily applied for the determination of compounds in human placental tissue samples collected at delivery from 25 randomly selected women. Copyright © 2015 Elsevier B.V. All rights reserved.

  14. FIA-Spectrophotometric Method for Determination of Nitrite in Meat Products: An Experiment Exploring Color Reduction of an Azo-Compound

    Science.gov (United States)

    Penteado, Jose C.; Angnes, Lucio; Masini, Jorge C.; Oliveira, Paulo C. C.

    2005-01-01

    This article describes the reaction between nitrite and safranine O. This sensitive reaction is based on the disappearance of color of the reddish-orange azo dye, allowing the determination of nitrite at the mg mL-1 level. A factorial optimization of parameters was carried out and the method was applied for the quantification of nitrite in…

  15. Improved determination of flavour compounds in butter by solid-phase (micro)extraction and comprehensive two-dimensional gas chromatography

    NARCIS (Netherlands)

    Adahchour, M.; Wiewel, J.; Verdel, R.; Vreuls, R.J.J.; Brinkman, U.A.T.

    2005-01-01

    The practicability and potential of comprehensive two-dimensional gas chromatography (GC × GC) coupled to both conventional flame ionisation (FID) and time-of-flight mass spectrometric (TOF-MS) detection, were compared with those of conventional one-dimensional (1D) GC, with the determination of

  16. Experimental Determination of pK[subscript a] Values and Metal Binding for Biomolecular Compounds Using [superscript 31]P NMR Spectroscopy

    Science.gov (United States)

    Swartz, Mason A.; Tubergen, Philip J.; Tatko, Chad D.; Baker, Rachael A.

    2018-01-01

    This lab experiment uses [superscript 31]P NMR spectroscopy of biomolecules to determine pK[subscript a] values and the binding energies of metal/biomolecule complexes. Solutions of adenosine nucleotides are prepared, and a series of [superscript 31]P NMR spectra are collected as a function of pH and in the absence and presence of magnesium or…

  17. Critical aspects in the determination of the antifouling compound dichlofluanid and its metabolite DMSA (N,N-dimethyl-N′-phenylsulfamide) in seawater and marine sediments

    NARCIS (Netherlands)

    Schouten, A.; Mol, H.; Hamwijk, C.; Ravensberg, J.C.; Schmidt, K.; Kugler, M.

    2005-01-01

    A straightforward method based on GC-MS was developed to determine the booster biocide dichlofluanid and its metabolite DMSA in sediment and water. Special attention was paid to conservation of samples, conversion of dichlofluanid to DMSA during analysis and the effect dichlofluanid-containing paint

  18. Devices for collecting chemical compounds

    Science.gov (United States)

    Scott, Jill R; Groenewold, Gary S

    2013-12-24

    A device for sampling chemical compounds from fixed surfaces and related methods are disclosed. The device may include a vacuum source, a chamber and a sorbent material. The device may utilize vacuum extraction to volatilize the chemical compounds from a fixed surface so that they may be sorbed by the sorbent material. The sorbent material may then be analyzed using conventional thermal desorption/gas chromatography/mass spectrometry (TD/GC/MS) instrumentation to determine presence of the chemical compounds. The methods may include detecting release and presence of one or more chemical compounds and determining the efficacy of decontamination. The device may be useful in collection and analysis of a variety of chemical compounds, such as residual chemical warfare agents, chemical attribution signatures and toxic industrial chemicals.

  19. Metabolic profiling and correlation analysis for the determination of killer compounds of proliferating and clonogenic HRT-18 colon cancer cells from Lafoensia pacari.

    Science.gov (United States)

    Reichert, Cristiane Loiva; da Silva, Denise Brentan; Carollo, Carlos Alexandre; Weffort-Santos, Almeriane Maria; de Moraes Santos, Cid Aimbiré

    2018-06-18

    Lafoensia pacari A. St.-Hil., belonging to the family Lythraceae and popularly known as 'dedaleira' and 'mangava-brava,' is a native tree of the Brazilian Cerrado, and its barks have been traditionally used as a tonic to treat inflammatory conditions, particularly related to gastric ulcers, wounds or fevers and various types of cancer. We have previously demonstrated the apoptogenic effects of the methanolic extract of L. pacari using various cancer cell lines. In the present study, this extract has been partitioned into fractions to identify the components that might be responsible for the apoptogenic effects using HRT-18 cells, which have been previously demonstrated to be sensitive to this extract. A standard methanolic extract was prepared and fractionated by centrifugal partition chromatography. The fractions were submitted to cytotoxicity and clonogenic assays to monitor the effects in parallel with LC-DAD-MS and statistical analyses to suggest the potential bioactive compounds. Besides ellagic acid, the primary constituent of the plant and also the biomarker of the species, one punicalin isomer, three pedunculagin I isomers, two castalagin isomers, three punicalagin HHDP-gallagyl-hexoside isomers, one ellagic acid deoxyhexose conjugate and one methyl ellagic acid deoxyhexose conjugate were putatively identified. The barks of L. pacari are rich in ellagic acid and various hydrolysable tannins, some of which were reported for the first time in this species, such as punicalagin and ellagitannins. This mixture of substances had the ability to kill proliferating cells and abrogate the growth of clonogenic cells in a similar manner shown by the methanolic extract of our previous study. The collective data reported herein suggest that the biological activities of the L. pacari barks used by the Cerrado's population to treat cancer conditions are due to the apoptogenic effects promoted by a mixed content of ellagitannins. Copyright © 2018. Published by Elsevier B.V.

  20. Synthesis and structure determination of the novel aluminophosphate TL-1: A new layered compound with corner-sharing AlX{sub 6} chains

    Energy Technology Data Exchange (ETDEWEB)

    Pastero, Linda [Dipartimento di Scienze della Terra, Università di Torino, Via Valperga Caluso 35, I-10125 Torino (Italy); Interdepartmental Centre “Nanostructured Interfaces and Surfaces-NIS”, Via Quarello 15A, 10135 Torino (Italy); CrisDi – Interdepartmental Center for Crystallography, Università di Torino, Via Pietro Giuria 7, I-10125 Torino (Italy); Arletti, Rossella, E-mail: rossella.arletti@unito.it [Dipartimento di Scienze della Terra, Università di Torino, Via Valperga Caluso 35, I-10125 Torino (Italy); Interdepartmental Centre “Nanostructured Interfaces and Surfaces-NIS”, Via Quarello 15A, 10135 Torino (Italy); CrisDi – Interdepartmental Center for Crystallography, Università di Torino, Via Pietro Giuria 7, I-10125 Torino (Italy); Cámara, Fernando [Dipartimento di Scienze della Terra, Università di Torino, Via Valperga Caluso 35, I-10125 Torino (Italy); Interdepartmental Centre “Nanostructured Interfaces and Surfaces-NIS”, Via Quarello 15A, 10135 Torino (Italy); CrisDi – Interdepartmental Center for Crystallography, Università di Torino, Via Pietro Giuria 7, I-10125 Torino (Italy); Gigli, Lara [Dipartimento di Scienze della Terra, Università di Torino, Via Valperga Caluso 35, I-10125 Torino (Italy); Interdepartmental Centre “Nanostructured Interfaces and Surfaces-NIS”, Via Quarello 15A, 10135 Torino (Italy); Cagnoni, Monica [Dipartimento di Chimica, Università di Torino, Via Pietro Giuria 7, I-10125 Torino (Italy)

    2016-10-15

    A novel layered aluminophosphate (TL-1) has been synthesized. Crystals grow as pseudo-hexagonal thin platelets and their whole morphology depends on the synthesis conditions. The structure was solved by single-crystal X-ray diffraction using charge flipping methods. The synthesized layered material, with composition [AlPO{sub 4}F(H{sub 2}O)]-(H{sub 10}C{sub 4}ON){sub 4}, crystallizes in the monoclinic space group P2{sub 1}/a with a=9.2282(5) Å, b=6.9152(4) Å, c=14.4615(9) Å, β=101.57(1)°. The novel compound has corner sharing AlO{sub 3}F{sub 2}(H{sub 2}O) octahedral chains running along [010], where fluorine atoms are at the shared apices, three oxygen atoms are shared with PO{sub 4} tetrahedra while the sixth oxygen pertain to an H{sub 2}O molecule. The stability field of the novel material is enclosed in the HF/Al{sub 2}O{sub 3} ratio ranging between 1 and 4 and the HF/morpholine ratio lower than 3. At temperature lower than 190 °C, the synthesis results is a pure aluminophosphate sample (low alumina/morpholine ratio). A treatment with H{sub 2}CO{sub 3} leads to a complete morpholine removal, as shown by in situ Raman spectroscopy. Powder X-ray diffraction reveals that, after morpholine extraction, the material collapses. The collapse is irreversible. - Highlights: • A new layered aluminophosphate was obtained and characterized. • The crystal structure is a sequence of aluminophosphate and organic layers. • The stability field of the new phase was defined by changing chemistry and T. • The templating agent can be removed by using a CO{sub 2} aqueous solution. • The decomposition of the morpholine induce a collapse in the structure.

  1. Development of methods for determining organic free radical structures by electron spin resonance and application to the radiation chemistry of nucleic acid model compounds

    International Nuclear Information System (INIS)

    Fouse, G.W. Jr.

    1977-01-01

    This project was undertaken with the objective of developing more efficient and reliable methods for the analysis of free radicals in organic single crystals. A technique was developed for the rapid calculation of single crystal ESR line positions and intensities. This method, which avoids the time-consuming matrix operations required by conventional methods, has been incorporated into a computer program for determining ESR parameters by the least-squares fitting of digitized ESR spectra. This program has been used to analyze complex spectra arising from a . CH 2 -CH 2 -O-PO 3 H - radical trapped in O-phosphorylethanolamine. A method was developed for the estimation of variance and covariance of eigenvectors and eigenvalues of experimentally-determined tensors. This error analysis is quite general, and may be applied to any tensors which can be determined by the non-linear least-squares fitting of ESR data. Monte-Carlo simulations have been employed to estimate the limitations of the approximation method. This error analysis has been included in the analysis of two phosphite radicals, - O 2 -P-OX, found in single crystals of O-phosphorylethanolamine. To aid in the formulation and evaluation of free radical models, a generalized method for the calculation of theoretically-expected hyperfine coupling tensors for arbitrary radical models was developed. Tensors are calculated for a furan-type radical which may be found in 5' dCMP. These calculated tensors are compared with tensors determined by an ENDOR experiment. Two ENDOR studies were done, one in 5' dCMP, the other in L-asparagine. The observed radical in 5' dCMP is allylic, characterized by coupling to three α-hydrogens. In L-asparagine, the dominant room-temperature radical has the form CO(NH 2 )CHCH(N + H 3 )CO 2 - . In both these studies, a series of molecular orbital calculations were performed as a means of substantiating the postulated radical structures

  2. Use of liquid chromatography for separation and determination of carrier species associated with the synthesis of no carrier-added sup(11)C labelled compounds

    International Nuclear Information System (INIS)

    Emran, Ali M.; Boothe, Th.E.; Finn, R.D.; Vora, M.M.; Kothari, P.J.

    1985-01-01

    An analytical technique using reversed-phase liquid chromatography was developed for the determination of urea at quantities as low as 1 ng to quantitate the amount of non-labelled urea produced during the synthesis of no-carrier-added [sup(11)C] urea starting from sup(11)CNsup(-). As a result, the specific activity of the [sup(11)C] urea thus prepared was calculated to be as high as 3.5+-0.8 Ci/μmol. (author)

  3. Simultaneous Determination of Four Compounds, Campesterol, Emodin8-O-β-D-Glucopyranoside, Quercetin, and Isoquercitrin in Reynoutria sachalinensis by High-performance Liquid Chromatography-Diode Array Detector

    Science.gov (United States)

    Eom, Min Rye; Weon, Jin Bae; Jung, Youn Sik; Ryu, Ga Hee; Yang, Woo Seung; Ma, Choong Je

    2017-01-01

    Background: Reynoutria sachalinensis is a well-known and used herbal medicine to treatment of arthralgia, jaundice, amenorrhea, coughs, carbuncles, and sores. Objective: We have developed high-performance liquid chromatography analysis method for simultaneous determination of isolated four compounds, campesterol, emodin8-O-β-D-glucopyranoside, quercetin, and isoquercitrin from R. sachalinensis is. Materials and Methods: The four compounds were separated on Shiseido C18 column (S-5 μm, 4.6 mm I.D. ×250 mm) at a column temperature of 25°C. The mobile phase composed of water and methanol with gradient elution system, and flow rate is 1.0 ml/min. The detection wavelength was set at 205 nm. Results: Validation of this analytical method was evaluated by linearity, precision, and accuracy test. This established method had good linearity (R2 > 0.997). The relative standard deviation values of intra- and inter-day testing were indicated that <2%, and accuracy is 91.66%–103.31% at intraday and 91.69%–103.31% at intraday. The results of recovery test were 92.60%–108.99%. Conclusion: In these results, developed method was accurate and reliable to the quality evaluation of campesterol, emodin 8-O-β-D-glucopyranoside, quercetin, and isoquercitrin isolated from R. sachalinensis. SUMMARY We have developed high-performance liquid analysis method for simultaneous determination of 4 compounds of Reynoutria sachalinensis. Abbreviations used: HPLC: High-performance liquid chromatography, DAD: Diode array detector, LOD: Limit of detection, LOQ: Limit of quantitation, ICH: International Conference on Harmonisation. PMID:28808389

  4. Determination of the torsion angles of alanine and glycine residues of model compounds of spider silk (AGG){sub 10} using solid-state NMR methods

    Energy Technology Data Exchange (ETDEWEB)

    Ashida, Jun; Ohgo, Kosuke; Komatsu, Kohei; Kubota, Ayumi; Asakura, Tetsuo [Tokyo University of Agriculture and Technology, Department of Biotechnology (Japan)], E-mail: asakura@cc.tuat.ac.jp

    2003-02-15

    Spiders synthesize several kinds of silk fibers. In the primary structure of spider silk, one of the major ampullate (dragline, frame) silks, spidroin 1, and flagelliform silk (core fibers of adhesive spiral), there are common repeated X-Gly-Gly (X = Ala, Leu, Pro, Tyr, Glu, and Arg) sequences, which are considered to be related to the elastic character of these fibers. In this paper, two dimensional spin diffusion solid-state NMR under off magic angle spinning (OMAS), {sup 13}C chemical shift contour plots, and Rotational Echo DOuble Resonance (REDOR) were applied to determine the torsion angles of one Ala and two kinds of Gly residues in the Ala-Gly-Gly sequence of {sup 13}C=O isotope-labeled (Ala-Gly-Gly){sub 10}. The torsion angles were determined to be ({phi}, {psi}) = (-90 deg., 150 deg.) within an experimental error of {+-}10 deg. for each residue. This conformation is characterized as 3{sub 1} helix which is in agreement with the structure proposed from the X-ray powder diffraction pattern of poly(Ala-Gly-Gly). The 3{sub 1} helix of (Ala-Gly-Gly){sub 10} does not change by formic acid treatment although (Ala-Gly){sub 15} easily changes from the silk I conformation (the structure of Bombyx mori silk fibroin before spinning in the solid state) to silk II conformation (the structure of the silk fiber after spinning) by such treatment. Thus, the 3{sub 1} helix conformation of (Ala-Gly-Gly){sub 10} is considered very stable. Furthermore, the torsion angles of the 16th Leu residue of (Leu-Gly-Gly){sub 10} were also determined as ({phi}, {psi}) = (-90 deg., 150 deg.) and this peptide is also considered to take 3{sub 1} helix conformation.

  5. Uses of complexone III and ion exchange resins in colorimetric determination with o-phenanthroline of Fe traces in uranium compounds

    International Nuclear Information System (INIS)

    Fernandez Cellini, R.; Ruiz Sanchez, F.

    1956-01-01

    The determination of small quantities of iron using o-phenanthroline, assumes the elimination of some cations interference by means of pH control before the formation of a coloured complex. We have eluded that difficulty by the connected action of complexones III and ion exchange. the previous forms quelate with the iron (III) with a stability constant high enough to permit the pass of an iron solution through a cation resin column without being fixed which never occurs with the interferer cations. Mercury is the only element with a similar stability, but it has been eliminated previously. (Author) 16 refs

  6. Isotopically modified compounds

    International Nuclear Information System (INIS)

    Kuruc, J.

    2009-01-01

    In this chapter the nomenclature of isotopically modified compounds in Slovak language is described. This chapter consists of following parts: (1) Isotopically substituted compounds; (2) Specifically isotopically labelled compounds; (3) Selectively isotopically labelled compounds; (4) Non-selectively isotopically labelled compounds; (5) Isotopically deficient compounds.

  7. The Onium Compounds

    Science.gov (United States)

    Tsarevsky, Nicolay V.; Slaveykova, Vera; Manev, Stefan; Lazarov, Dobri

    1997-06-01

    The onium salts are of a big interest for theoretical and structural chemistry, and for organic synthesis. Some representatives of the group (e.g. ammonium salts) were known from the oldest times. Many onium salts are met the nature: ammonium salts (either as inorganic salts, and organic derivatives, e.g. aminoacids, salts of biogenic amines and alkaloids, etc.); oxonium salts (plant pigments as anthocyans are organic oxonium compounds), etc. In 1894 C. Hartmann and V. Meyer prepared the first iodonium salts - 4-iododiphenyliodonium hydrogensulfate and diphenyliodonium salts, and suggested the ending -onium for all compounds with properties similar to those of ammonium salts. Nowadays onium compounds of almost all nonmetals are synthesised and studied. A great variety of physical methods: diffraction (e.g. XRD) and spectral methods (IR-, NMR-, and UV-spectra), as well as the chemical properties and methods of preparation of onium salts have been used in determination of the structure of these compounds. The application of different onium salts is immense. Ammonium, phosphonium and sulfonium salts are used as phase-transfer catalysts; diazonium salts - for the preparation of dyes, metalochromic and pH-indicators. All the onium salts and especially diazonium and iodonium salts are very useful reagents in organic synthesis.

  8. Development of a method for analyzing traces of ruthenium in plant materials and determination of the transfer factors soil/plant for ruthenium compounds from reprocessing plants

    International Nuclear Information System (INIS)

    Blasius, E.; Huth, R.; Neumann, W.

    1988-01-01

    In an artificial humous and sandy soil spiked with 106 Ru as RuO 2 and RuCl 3 , pasture grass was grown under artificial illumination in our laboratory. The amounts of ruthenium taken up by the plants were determined by γ-spectrometry. For open-air investigations with pasture grass, wheat and potatoes inactive ruthenium(III) chloride and ruthenium nitrosylchloride were used. Ruthenium was determined by electrothermal atomic absorption spectrometry (ETAAS) after destroying the organic material and concentrating the solution. The concentration and chemical form of the ruthenium exert an unimportant influence on the transfer factor. For the pasture-grass, the stems of wheat and the weed of potatoes it amounts to 0.00005 to 0.0015, for the ear of wheat to about 0.00005. In peeled potatoes there was no ruthenium detectable, therefore the limit of detection leads to a transfer factor ≤ 0.00001. So it is evident that ruthenium is little available for the roots of the plants. In the event of an accident in a nuclear plant the uptake of radioactive ruthenium by roots has only negligible radioecological consequences. This applies even if 50 years of ruthenium enrichment in the soil are assumed. (orig./RB)

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

    Directory of Open Access Journals (Sweden)

    H. A. Mashayekhi

    2014-09-01

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

  10. Application of correlation constrained multivariate curve resolution alternating least-squares methods for determination of compounds of interest in biodiesel blends using NIR and UV-visible spectroscopic data.

    Science.gov (United States)

    de Oliveira, Rodrigo Rocha; de Lima, Kássio Michell Gomes; Tauler, Romà; de Juan, Anna

    2014-07-01

    This study describes two applications of a variant of the multivariate curve resolution alternating least squares (MCR-ALS) method with a correlation constraint. The first application describes the use of MCR-ALS for the determination of biodiesel concentrations in biodiesel blends using near infrared (NIR) spectroscopic data. In the second application, the proposed method allowed the determination of the synthetic antioxidant N,N'-Di-sec-butyl-p-phenylenediamine (PDA) present in biodiesel mixtures from different vegetable sources using UV-visible spectroscopy. Well established multivariate regression algorithm, partial least squares (PLS), were calculated for comparison of the quantification performance in the models developed in both applications. The correlation constraint has been adapted to handle the presence of batch-to-batch matrix effects due to ageing effects, which might occur when different groups of samples were used to build a calibration model in the first application. Different data set configurations and diverse modes of application of the correlation constraint are explored and guidelines are given to cope with different type of analytical problems, such as the correction of matrix effects among biodiesel samples, where MCR-ALS outperformed PLS reducing the relative error of prediction RE (%) from 9.82% to 4.85% in the first application, or the determination of minor compound with overlapped weak spectroscopic signals, where MCR-ALS gave higher (RE (%)=3.16%) for prediction of PDA compared to PLS (RE (%)=1.99%), but with the advantage of recovering the related pure spectral profile of analytes and interferences. The obtained results show the potential of the MCR-ALS method with correlation constraint to be adapted to diverse data set configurations and analytical problems related to the determination of biodiesel mixtures and added compounds therein. Copyright © 2014 Elsevier B.V. All rights reserved.

  11. Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of semivolatile organic compounds in bottom sediment by solvent extraction, gel permeation chromatographic fractionation, and capillary-column gas chromatography/mass spectrometry

    Science.gov (United States)

    Furlong, E.T.; Vaught, D.G.; Merten, L.M.; Foreman, W.T.; Gates, Paul M.

    1996-01-01

    A method for the determination of 79 semivolatile organic compounds (SOCs) and 4 surrogate compounds in soils and bottom sediment is described. The SOCs are extracted from bottom sediment by solvent extraction, followed by partial isolation using high-performance gel permeation chromatography (GPC). The SOCs then are qualitatively identified and quantitative concentrations determined by capillary-column gas chromatography/mass spectrometry (GC/MS). This method also is designed for an optional simultaneous isolation of polychlorinated biphenyls (PCBs) and organochlorine (OC) insecticides, including toxaphene. When OCs and PCBs are determined, an additional alumina- over-silica column chromatography step follows GPC cleanup, and quantitation is by dual capillary- column gas chromatography with electron-capture detection (GC/ECD). Bottom-sediment samples are centrifuged to remove excess water and extracted overnight with dichloromethane. The extract is concentrated, centrifuged, and then filtered through a 0.2-micrometer polytetrafluoro-ethylene syringe filter. Two aliquots of the sample extract then are quantitatively injected onto two polystyrene- divinylbenzene GPC columns connected in series. The SOCs are eluted with dichloromethane, a fraction containing the SOCs is collected, and some coextracted interferences, including elemental sulfur, are separated and discarded. The SOC-containing GPC fraction then is analyzed by GC/MS. When desired, a second aliquot from GPC is further processed for OCs and PCBs by combined alumina-over-silica column chromatography. The two fractions produced in this cleanup then are analyzed by GC/ECD. This report fully describes and is limited to the determination of SOCs by GC/MS.

  12. Determination of linuron and related compounds in soil by microwave-assisted solvent extraction and reversed-phase liquid chromatography with UV detection.

    Science.gov (United States)

    Molins, C; Hogendoorn, E A; Dijkman, E; Heusinkveld, H A; Baumann, R A

    2000-02-11

    The combination of microwave-assisted solvent extraction (MASE) and reversed-phase liquid chromatography (RPLC) with UV detection has been investigated for the efficient determination of phenylurea herbicides in soils involving the single-residue method (SRM) approach (linuron) and the multi-residue method (MRM) approach (monuron, monolinuron, isoproturon, metobromuron, diuron and linuron). Critical parameters of MASE, viz, extraction temperature, water content and extraction solvent were varied in order to optimise recoveries of the analytes while simultaneously minimising co-extraction of soil interferences. The optimised extraction procedure was applied to different types of soil with an organic carbon content of 0.4-16.7%. Besides freshly spiked soil samples, method validation included the analysis of samples with aged residues. A comparative study between the applicability of RPLC-UV without and with the use of column switching for the processing of uncleaned extracts, was carried out. For some of the tested analyte/matrix combinations the one-column approach (LC mode) is feasible. In comparison to LC, coupled-column LC (LC-LC mode) provides high selectivity in single-residue analysis (linuron) and, although less pronounced in multi-residue analysis (all six phenylurea herbicides), the clean-up performance of LC-LC improves both time of analysis and sample throughput. In the MRM approach the developed procedure involving MASE and LC-LC-UV provided acceptable recoveries (range, 80-120%) and RSDs (<12%) at levels of 10 microg/kg (n=9) and 50 microg/kg (n=7), respectively, for most analyte/matrix combinations. Recoveries from aged residue samples spiked at a level of 100 microg/kg (n=7) ranged, depending of the analyte/soil type combination, from 41-113% with RSDs ranging from 1-35%. In the SRM approach the developed LC-LC procedure was applied for the determination of linuron in 28 sandy soil samples collected in a field study. Linuron could be determined in

  13. Development and validation of High-performance Thin-layer Chromatography Method for Simultaneous Determination of Polyphenolic Compounds in Medicinal Plants.

    Science.gov (United States)

    Jayachandran Nair, C V; Ahamad, Sayeed; Khan, Washim; Anjum, Varisha; Mathur, Rajani

    2017-12-01

    Quantitative standardization of plant-based products is challenging albeit essential to maintain their quality. This study aims to develop and validate high-performance thin-layer chromatography (HPTLC) method for the simultaneous determination of rutin (Ru), quercetin (Qu), and gallic acid (Ga) from Psidium guajava Linn. (PG) and Aegle marmelos (L.) Correa. (AM) and correlate with antioxidant activity. The stock solution (1 mg/mL) of standard Ru, Qu, and Ga in methanol: Water (1:1) was serially diluted and spotted (5 μL) on slica gel 60 F 254 thin-layer chromatography plates. Toluene: Ethyl acetate: Formic acid: Methanol (3:4:0.8:0.7, v/v/v) was selected as mobile phase for analysis at 254 nm. Hydroalcoholic (1:1) extracts of leaves of PG and AM were fractionated and similarly analyzed. Antioxidant activity was also determined using 2, 2-diphenyl-1-picrylhydrazyl assay. The developed method was robust and resolved Ru, Qu, and Ga at R f 0.08 ± 0.02, 0.76 ± 0.01, and 0.63 ± 0.02, respectively. The intra-day, interday precision, and interanalyst were limit of detection and limit of quantification for Ru, Qu, and Ga were 4.51, 4.2, 5.27, and 13.67, 12.73, 15.98 ng/spot, respectively. Antioxidant activity (Log 50% inhibition) of PG and AM was 4.947 ± 0.322 and 6.498 ± 0.295, respectively. The developed HPTLC method was rapid, accurate, precise, reproducible, and specific for the simultaneous estimation of Ru, Qu, and Ga. HPTLC method for simultaneous determination and quantification of Rutin, Quercetin and Gallic acid, is reported for quality control of herbal drugs. Abbreviations Used: A: Aqueous fraction; AM: Aegle marmelos L. Correa; B: Butanol fraction; C: Chloroform fraction; EA: Ethyl acetate fraction; Ga: Gallic acid; H: Hexane fraction; HA: Hydroalcoholic extract; HPTLC: High-performance thin-layer chromatography; PG: Psidium guajava ; Qu: Quercetin; Ru: Rutin.

  14. Transfer of pharmacopoeial liquid chromatography reversedphase methods for determination of related compounds in diclofenac sodium and metamizole sodium from conventional to core-shell column

    Directory of Open Access Journals (Sweden)

    Katerina Brezovska

    2015-04-01

    Full Text Available Core-shell silica particles were developed as a new material for chromatographic stationary phases in order to provide fast and high efficiency separations of small and large molecules and complex samples, at pressures compatible with conventional HPLC equipment. The aim of our work was to show the applicability of the HPLC columns based on a core-shell technology for determination of related substances in diclofenac sodium and in metamizole sodium using the methods described in the corresponding monographs of the European pharmacopoeia. The obtained results have shown that the proposed methods can be successfully transferred on core shell column, with suitable adjustment of injection volume and flow rate. The advantage of using core-shell column is fast and highly efficient separation on conventional HPLC equipment with increased sensitivity of the method and high throughput of the analysis, providing enhanced lab productivity and reduced costs.

  15. Determination of slip systems and their relation to the high ductility and fracture toughness of the B2 DyCu intermetallic compound

    International Nuclear Information System (INIS)

    Cao, G.H.; Shechtman, D.; Wu, D.M.; Becker, A.T.; Chumbley, L.S.; Lograsso, T.A.; Russell, A.M.; Gschneidner, K.A.

    2007-01-01

    DyCu single crystals with CsCl-type B2 structure were tensile tested at room temperature. Slip trace analysis shows that the primary slip system in DyCu with a tensile axis orientation of is {1 1 0} and the critical resolved shear stress for {1 1 0} slip is 18 MPa. Slip traces were also observed from a secondary slip system, {1 1 0} , and this slip system appears to be a key contributor to the previously reported high ductility and high fracture toughness of polycrystalline DyCu. Transmission electron microscopy determinations of the Burgers vectors of dislocations in tensile tested specimens revealed and dislocations, with -type dislocations being more abundant. The implications of these findings for the understanding of the mechanical properties of DyCu and the large family of ductile rare earth B2 intermetallics are discussed

  16. Compounds interaction on biodegradation of toluene and methyl ...

    African Journals Online (AJOL)

    MEK) mixtures in a composite bead biofilter was investigated. The biodegradation rate of two compounds in the exponential growth phase and stationary phase for the single compound and two compounds mixing systems was determined.

  17. Screening of metabolites secondary compounds in extract of moringa fruit and determination of inhibitory effect on growth of the fungus Candida albicans

    Science.gov (United States)

    Nuryanti, Siti; Puspitasari, Dwi Juli

    2017-08-01

    Moringa (Moringa oleifera Lamk) is a nutritious plant that can cure various diseases. Parts of this plant like leave, root, flower, and fruit can be used as a traditional medicine. The research about screening of secondary metabolites in moringa extracts and the determination of their inhibitory effect on growth of the fungus Candida albicans have been done. This research was conducted by extracting the moringa fruit with various solvent with different polarity namely hexane, distilled water and ethanol. The fungal inhibition test was done by well-difuse method. Suspensions of Candida albicans was standardized by 0.5 Mc Farland standard. The results showed that the extracts of Moringa with distilled water provided the greatest inhibition on the growth of the fungus Candida albicans compared to moringa fruit extracted by ethanol and hexane. The percentages inhibition of Moringa extracts on the growth of the Candida albicans with distilled water, ethanol and hexane solvents were 89.90%, 57.90% and 8.97% respectively. Phytochemical screening test showed that the moringa fruit contain alkaloids, flavonoids and steroids.

  18. Determination of thiol compounds by solid-phase extraction using multi-walled carbon nanotubes as adsorbent coupled with high-performance liquid chromatography-fluorescence detection

    International Nuclear Information System (INIS)

    Huang, K.J.; Han, C.H.; Han, C.Q.; Li, J.; Wu, Z.W.; Liu, Y.M.

    2011-01-01

    We describe a method for solid-phase extraction of biogenic thiols using multi-walled carbon nanotubes as adsorbent, and their subsequent determination via HPLC and fluorescence detection. The fluorogenic reagent N-(4,4-difluoro-5,7-dimethyl-4-bora-3a,4a-diaza-s-indacene-3-yl)methyl) iodoacetamide was applied to derivatizate the thiols. The type of eluent and its volume, the sample pH, extraction time and sample volume were optimized. The calibration curves of the thiols are linear in the range from 0. 5 to 200 nM (for glutathione), 0. 02 to 5 nM (for cysteine), and 2 to 500 nM (for acetylcysteine), and the correlation coefficients range between 0. 9955 and 0. 9997. The respective limits of detection are 20 pM, 4 pM and 80 pM (at an SNR of 3), and the limits of quatification are 67 pM, 13 pM, and 267 pM (at an SNR of 10). Recoveries range from 85.0% to 113.1% for human urine and plasma samples spiked with the three thiols, and relative standard deviations are in the range from 2.1 to 7.4%. (author)

  19. Determination of contents and antioxidant activity of free and bound phenolics compounds and in vitro digestibility of commercial black and red rice (Oryza sativa L.) varieties.

    Science.gov (United States)

    Sumczynski, Daniela; Kotásková, Eva; Družbíková, Helena; Mlček, Jiří

    2016-11-15

    Black and red rices (Oryza sativa L.) were analysed for total flavonoids and phenolics and the HPLC profile including both free and bound phenolic fractions. Moreover, antioxidant activity and in vitro digestibility was determined. Content of flavonoids and polyphenols as well as antioxidant activity was higher in free phenolic fractions. Bound flavonoids in black rices were not significant contributors to antioxidant activity. The main free phenolics in black rices were ferulic, protocatechuic and trans-p-coumaric acids, while the major free phenolics in red rices were catechin, protocatechuic and caffeic acids. The main bound phenolics in black rices were ferulic and vanillic acids and quercetin, in red rice types, they were ferulic, syringic, trans-p-coumaric acids and quercetin. Newly, the presence of m-coumaric acid in red rices was detected. Steam cooked rices showed very high levels of organic matter digestibility, whereas red rices were significantly more digestible than black rices (p<0.05). Copyright © 2016 Elsevier Ltd. All rights reserved.

  20. Determining the pk(a) of N,N-dimethylsphingosine and the flip-flop rate of related compounds with deuterium nuclear magnetic resonance

    International Nuclear Information System (INIS)

    Lau, Bienca

    1995-01-01

    Deuterium nuclear magnetic resonance ( 2 H-NMR) spectroscopy was applied to determine the pk(a) of the protein kinase C (PKC) inhibitor, N,N-dimethylsphingosine (DMS), when bound to 1-palmitoyl-2-oleoyl-sn-glycero-3-phosphocholine (POPC) bilayers. The quadrupolar splittings from deuterium labels at the α- and the β-positions of the POPC headgroup responded in a manner indicative of a positive surface charge density at pH 7.0. Conversely, at pH 10.0 DMS had virtually no influence on either quadrupolar splitting, an effect attributed to titration of the dimethylamino group of DMS to its neutral form. A DMS titration curve was obtained by quantifying the charge in the quadrupolar splittings as a function of pH. Simulation of this curve yielded a pk(a) of 8.8 of membrane-bound DMS. Using a similar approach, the dynamic process of flip-flop was examined in two DMS analogues. We discuss here the quantitative and the qualitative aspects as well as the limitations of this application. (author)