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311.
Two samples of mussels (Mytilus edulis) were collected from the southwest of Ireland. One sample contained domoic acid, the other sample contained okadaic acid,
dinophysistoxin-2 and azaspiracid-1, -2 and -3. Wet and freeze-dried reference materials were prepared from each of the two
samples to test for differences in homogeneity, stability and extractability of the analytes in either condition. Wet materials
were homogenised, aliquoted and hermetically sealed under argon and subsequently frozen at −80 °C. Dry materials were similarly
homogenised but frozen in flat cakes prior to freeze-drying. After grinding, sieving and further homogenisation, the resulting
powder was aliquoted and hermetically sealed. Domoic acid materials were characterised using HPLC–UV, while LC–MS was used
for the determination of lipophilic toxins. The extractabilities of all phycotoxins studied were comparable for wet and freeze-dried
materials once a sonication step had been carried out for reconstitution of the freeze-dried materials prior to extraction.
Homogeneity was assessed through replicate analysis of the phycotoxins (n = 10), and was found to be similar for wet and freeze-dried materials, for both hydrophilic and lipophilic toxins. Water
contents were determined for both wet and freeze-dried materials, and particle size was determined for the freeze-dried materials.
Stability was evaluated isochronously over eight months at four temperatures (−20, +4, +20 and +40 °C). The freeze-dried material
containing domoic acid was stable over the whole duration at all temperatures, while in the wet material domoic acid degraded
to some extent at all temperatures except −20 °C. In freeze-dried and wet materials containing lipophilic toxins, okadaic
acid, dinophysistoxin-2, azaspiracid-1 and azaspiracid-2 were stable over the whole duration at all conditions, while concentrations
of azaspiracid-3 changed significantly in both materials at some storage temperatures.
Figure Aliquots of freeze-dried and wet mussel tissue reference materials containing the various shellfish toxins examined in the
study 相似文献
312.
Microwave-assisted thermal desorption (MAD) coupled to headspace solid-phase microextraction (HS-SPME) has been studied for
in-situ, one-step, sample preparation for PAHs collected on XAD-2 adsorbent, before gas chromatography with mass spectrometric
detection. The PAHs on XAD-2 were desorbed into the extraction solution, evaporated into the headspace by use of microwave
irradiation, and absorbed directly on a solid-phase microextraction fiber in the headspace. After desorption from the SPME
fiber in the hot GC injection port, PAHs were analyzed by GC–MS. Conditions affecting extraction efficiency, for example extraction
solution, addition of salt, stirring speed, SPME fiber coating, sampling temperature, microwave power and irradiation time,
and desorption conditions were investigated. Experimental results indicated that extraction of 275 mg XAD-2, containing 10–200 ng
PAHs, with 10-mL ethylene glycol–1 mol L−1 NaCl solution, 7:3, by irradiation with 120 W for 40 min (the same as the extraction time), and collection with a PDMS–DVB
fiber at 35 °C, resulted in the best extraction efficiency. Recovery was more than 80% and RSD was less than 14%. Optimum
desorption was achieved by heating at 290 °C for 5 min. Detection limits varied from 0.02 to 1.0 ng for different PAHs. A
real sample was obtained by using XAD-2 to collect smoke from indoor burning of joss sticks. The amounts of PAHs measured
varied from 0.795 to 2.53 ng. The method is a simple and rapid procedure for determination of PAHs on XAD-2 absorbent, and
is free from toxic organic solvents. 相似文献
313.
The aim of this work was to establish optimal conditions for the maximum production of endo-β-1,4 mannanases using cheaper
sources. Eight thermotolerant fungal strains were isolated from garden soil and compost samples collected in and around the
Gulbarga University campus, India. Two strains were selected based on their ability to produce considerable endo-β-1,4 mannanases
activity while growing in liquid medium at 37 °C with locust bean gum (LBG) as the only carbon source. They were identified
as Aspergillus niger gr and Aspergillus flavus gr. The experiment to evaluate the effect of different carbon sources, nitrogen sources, temperatures and initial pH of the
medium on maximal enzyme production was studied. Enzyme productivity was influenced by the type of polysaccharide used as
the carbon source. Copra meal defatted with n-hexane showed to be a better substrate than LBG and guar gum for endo-β-1,4 mannanases production by A. niger gr (40.011 U/ml), but for A. flavus gr (33.532 U/ml), the difference was not significant. Endo-β-1,4 mannanases produced from A. niger gr and A. flavus gr have high optimum temperature (65 and 60 °C) and good thermostability in the absence of any stabilizers (maintaining 50%
of residual activity for 8 and 6 h, respectively, at 60 °C) and are stable over in a wide pH range. These new strains offer
an attractive alternative source of enzymes for the food and feed processing industries. 相似文献
314.
Wang F Weidt S Xu J Mackay CL Langridge-Smith PR Sadler PJ 《Journal of the American Society for Mass Spectrometry》2008,19(4):544-549
Reactions of the anticancer complex [(eta(6)-bip)Ru(en)Cl](+) (where bip is biphenyl and en is ethylenediamine) with the tripeptide glutathione (gamma-L-Glu-L-Cys-Gly; GSH), the abundant intracellular thiol, in aqueous solution give rise to two ruthenium cluster complexes, which could not be identified by electrospray mass spectrometry (ESI-MS) using a quadrupole mass analyzer. Here we use Fourier transform ion cyclotron mass spectrometry (nanoLC-FT-ICR MS) to identify the clusters separated by nanoscale liquid chromatography as the tetranuclear complex [{(eta(6)-bip)Ru(GSO(2))}(4)](2-) (2) and dinuclear complex [{(eta(6)-bip)Ru(GSO(2))(2)}(2)](8-) (3) containing glutathione sulfinate (GSO(2)) ligands. Use of (18)OH(2) showed that oxygen from water can readily be incorporated into the oxidized glutathione ligands. These data illustrate the power of high-resolution MS for identifying highly charged multinuclear complexes and elucidating novel reaction pathways for metallodrugs, including ligand-based redox reactions. 相似文献
315.
Using Stuttgart/Dresden effective core potentials MWB28, MWB60, and GTO valence basis sets (8s7p6d)/[6s5p3d], (8s7p6d)/[6s5p3d]
for Zr and Hf atoms and 6-311++G(3df,3pd) basis set for C, H, O, and Ti atoms, tight convergence criteria geometry optimizations
and harmonic frequency calculations are performed at B3LYP and B3LYP/IEF-PCM levels of theory so as to model the gas phase
and argon matrix infrared spectra of the tetrahedral molecules R2MH2 (R = D(H), CH3, OH; M = Ti, Zr, Hf). Influence of the transition metal and/or substituent group on the symmetric and asymmetric stretching
frequencies of the MH2 fragment of the R2MH2 molecules is investigated at both the levels of theory. The modelling of the argon matrix effect improves the agreement between
the calculated frequencies and the experimental ones. The calculated argon matrix to gas phase frequency shifts is compared
reasonably to the experimental argon to neon matrix shifts. 相似文献
316.
A. Varesano C. Tonin F. Ferrero Marinella Stringhetta 《Journal of Thermal Analysis and Calorimetry》2008,94(2):559-565
Electro-conducting doped polypyrrole was deposited by in situ oxidative polymerisation on PET non-wovens. Thermal properties were evaluated by means of DSC and TG in nitrogen and air.
Flame resistance tests reveal that coated PET fibres resist to direct contact with fire. By thermal analysis, it was found
that PPy reduces the temperature at which thermo-oxidative degradation of PET occurs. Polypyrrole-coated PET non-wovens were
heated above the melting point of PET for 30 min. After the heating the fibres become brittle and frail, but SEM observations
revealed that they maintained their fibrous shape. A loss of chlorine was found because of intense heating. 相似文献
317.
3,5-Bis(2-hydroxyphenyl)-1H-1,2,4-triazole (H2La) and 4-[3,5-bis(2-hydroxyphenyl)-1H-1,2,4-triazol-1-yl]benzoic acid (H3Lb) have been prepared, and crystal structure of the intermediate 2-(2-hydroxyphenyl)-4H-1,3-benzoxazin-4-one has been determined. Temperature dependent 1H NMR spectroscopic measurements of H2La indicated dynamic behavior with the equilibrium between the two asymmetric tautomers. For H3Lb, pD-dependent 1H NMR spectroscopic measurements showed small but characteristic shifts in the range of 0 ≤ pD ≤ 1, indicative of a triazole
nitrogen atom protonation; the corresponding pK
a of 0.98 ± 0.04 was determined by spectrophotometric titrations. (H2O, 26°C, 1 M KCl/HCl). Formation of [FeIII(La)]+ (pH 2.5) and [FeIII(La)2]− (pH > 6) was verified by UV-Vis spectroscopy. Complex formation of H3Lb with Al3+ and VO2+ was investigated by 1H NMR spectroscopic titration and cyclic voltammetry, respectively. Single crystals of the phenoxo bridged [VVO(HLb)(EtO)]2·2EtOH were characterized by X-ray structural analysis.
Dedicated to Professor Milan Melník on the occasion of his 70th birthday 相似文献
318.
Borjana V. Donkova Katja I. Milenova Dimitar R. Mehandjiev 《Central European Journal of Chemistry》2008,6(1):115-124
The precursors with a low manganese content ≤ 0.07% Mn were synthesized by spontaneous crystallization from Zn2+, Mn2+ and C2O4
2−-containing solutions. The initial ratio Zn2+:C2O4
2− = 1:1 and 1:2 influences the morphology and prevailing orientations of the crystallites in the oxalate samples. The presence
of such small Mn content in the samples does not change the morphology or size of the crystals. The ZnO and Mn/ZnO oxides
with manganese content from 0.51×10−2 to 15.1×10−2 Wt % are obtained after thermal decomposition of the oxalates. The oxides preserved the morphology of the precursors. The
catalytic tests show that the pure ZnO has a poor activity for CO oxidation reaction. Its doping with Mn promotes the catalytic
activity (up from twice to five times) in spite of the very low contents of the dopants. The observed increase of the activity
depends on both dopant concentration and Zn2+:C2O4
2− ratio, probably due to the different mechanism of the manganese inclusion and different morphology of the oxides. The catalysts
of the 1:2 series are more active in CO oxidation reaction.
相似文献
319.
Sun YX Huang YX Li FL Wang HY Fan C Bao YL Sun LG Ma ZQ Kong J Li YX 《Chemistry Central journal》2012,6(1):2
Background
The virtual screening (VS) of lead compounds using molecular docking and pharmacophore detection is now an important tool in drug discovery. VS tasks typically require a combination of several software tools and a molecular graphics system. Thus, the integration of all the requisite tools in a single operating environment could reduce the complexity of running VS experiments. However, only a few freely available integrated software platforms have been developed. 相似文献320.
Yazhou Wang Lixin Wang Zhipeng Ma Lijun Gao Xucai Yin Ailing Song Xiujuan Qin Guangjie Shao Weimin Gao 《Journal of Solid State Electrochemistry》2018,22(10):2977-2987
MnO has a high theoretical capacity, moderate discharge plateau, and low polarization when it is used as the anode material in lithium battery. However, the issues that limit its application are its poor conductivity and large volume changes, which can easily result in the collapse of electrode structure during long-term cycling. In the present work, a carbon-coated MnO/graphene 3D-network anode material is synthesized by an electrostatic adsorption of dispersed precipitates precipitation method. The MnO nanoparticles coated by carbon are uniformly distributed on the surface of graphene nanosheets and form a 3D sandwich-like nanostructure. A carbon layer is coated on the surface of MnO nanoparticles, which slows down the volume expansion in the process of lithium intercalation. The graphene nanosheets are cross-linked through carbons in this 3D nanostructure, which provides mechanical support and effective electron conduction pathways during the charge-discharge. The electrochemical tests indicate that the prepared 3D carbon-coated MnO/graphene electrode exhibits an excellent rate capacity of 1247.3 and 713.2 mAh g?1 at 100 and 1000 mA g?1, respectively. The capacity is 792.2 mAh g?1 after long cycle at a current density of 1000 mA g?1. The specific capacity is higher than that of MnO-based composite lithium anode materials currently reported. The superior rate and cycling performances are attributed to the unique 3D-network structure, which provides an effectively conductive network, buffers volume expansion, and prevents falling and aggregation of MnO in the charge and discharge process of the electrode materials. The 3D-structured carbon-coated MnO/graphene anode material will have an excellent application prospect. 相似文献