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121.
Phoebe Y. T. Hon Man-ying Wan Della W. M. Sin Yiu-chung Wong 《Analytical and bioanalytical chemistry》2013,405(23):7241-7250
This paper describes a metrological approach to evaluate the measurement capability of laboratories participating in two proficiency testing (PT) programmes involving the analysis of five polycyclic aromatic hydrocarbons (PAHs) in sediment samples. Reference values of PAHs in the programmes for performance assessment were obtained from an accurate isotope dilution gas chromatography mass spectrometry (ID-GCMS) method which was thoroughly validated and verified. Isotope dilution mass spectrometry (IDMS) technique usually has a well-defined measurement uncertainty budget and a traceability link to an International System of Units. Provision of the metrological reference values in PT enables the establishment of a technical platform to assess the actual competence of the participating laboratories in sediment PAHs analysis. Results of the PT programmes showed that about 80 % of the laboratories employed gas chromatography in their analyses and the remaining used liquid chromatography. Irrespective of the techniques being used, however, the majority of the participating laboratories were observed to underestimate values in which the mean values of the five reported PAHs were less than those of the ID-GCMS-derived reference values by 13–20 %. Only 41–44 % of the participating laboratories were able to achieve satisfactory z-scores. The present study revealed that the reinforcement of the capability for accurate measurement of PAHs in sediment samples in laboratories worldwide should be addressed. 相似文献
122.
Dadan Hermawan Izdiani Mohd Yatim Khaulah Ab Rahim Mohd Marsin Sanagi Wan Aini Wan Ibrahim Hassan Y. Aboul-Enein 《Chromatographia》2013,76(21-22):1527-1536
A simple solid phase extraction (SPE) method coupled with high performance liquid chromatography (HPLC) using UV detector and microemulsion electrokinetic chromatography (MEEKC) has been developed and compared for the quantitative determination of miconazole nitrate in pharmaceutical formulation. For HPLC method, two parameters were optimized, namely, the wavelength and the mobile phases. The optimized condition was at the 225 nm wavelength and the mobile phase of ACN:MeOH (90:10 v/v). There are seven MEEKC parameters that were optimized, in this research, which were applied to voltage, temperature, wavelength, sodium dodecyl sulfate (SDS) concentration, buffer pH, buffer concentration and butan-1-ol concentration. The optimum MEEKC condition was obtained using 86.35 % (w/w) 2.5 mM borate buffer pH 9, 0.25 % (w/w) SDS, 0.8 % (w/w) ethyl acetate, 6.6 % w/w butan-1-ol and 6.0 % (w/w) acetonitrile. The combination of SPE using a diol column with HPLC–UV and the MEEKC methods were successfully applied for the determination of miconazole nitrate in a pharmaceutical formulation with the recovery percentage of 98.35 and 92.50 %, respectively. 相似文献
123.
Characterization of Nitro-Substituted Polybenzimidazole Synthesized by the Reaction with Nitric Acid
Abstract Nitro-substituted poly[2,2′-(m-phenylene)-5,5′-bibenzimidazole]s (PBIs) were synthesized by the reaction of PBI with nitric acid in sulfuric acid under various conditions. The number of nitro groups substituted on the aromatic ring of PBI per polymeric unit varied from 1.44 to 3.55 according to the reaction conditions. An increase in reaction temperature and concentration of the nitric acid increased the degree of substitution. The inherent viscosity of the substituted polymer increased as the reaction temperature decreased. When the reaction temperature was 30°C, the inherent viscosity of the polymer increased as the concentration of nitric acid increased. The nitro-substituted PBI exhibited polyelectrolyte behavior in formic acid. The nitro groups substituted on PBI were dissociated when the polymer was heated to 450°C, displaying exothermic behavior, and the decomposition of polymer was proportional to its nitro group content. All nitro-substituted PBIs showed better solubilities in polar aprotic and acidic solvents, such as dimethylacetamide, dimethylsulfoxide, dimethylformamide, N-methylpyrrolidone, formic acid, sulfuric acid, and trifluoromethanesulfonic acid. 相似文献
124.
Trenbolone (TRE) is a steroid used by veterinarians on livestock to increase appetite and body weight. The use of TRE has been restricted because of its harmful side effect for consumers. To effectively control TRE residue in food and food product, a rapid and convenient immunoassay was developed by preparing an anti-TRE monoclonal antibody. The immunogen and coating antigen were prepared by coupling TRE hapten with carrier proteins via 1-ethyl-3-(dimethylaminopropyl)carbodiimide hydrochloride (EDC) method. The optimized method gave an average IC50 value of 0.323 ng mL−1 towards TRE and an average detection limit (LOD) of 0.06 ng mL−1, which is much lower than the maximum residue levels (2.0 ng g−1) accepted by the Joint FAO/WHO Expert Committee on Food Additives (JECFA). The specificity of the antibody was evaluated by measuring cross-reactivity of six structurally related compounds, including 19-nortestosterone (9.7%), testosterone (0.13%), methyltestosterone (<0.01%), methandrostenolone (<0.01%), (+)-dehydroisoandrosterone (<0.001%) and β-estradiol (<0.001%). The recovery rates of the test in detection of TRE-fortified animal tissue, urine and animal feed samples were in the range of 81.3-89.4%, while the intra- and inter-assay coefficients of variation were less than 12.0%. 相似文献
125.
Wang W Wang HY Wei W Xiao ZG Wan Y 《Chemistry (Weinheim an der Bergstrasse, Germany)》2011,17(48):13461-13472
We demonstrate the self-assembling and size-selective synthesis of uniform and highly dispersed Ni or NiO nanoparticles with diameters below 12 nm embedded in ordered mesoporous carbon or polymer frameworks. Self-assembly is induced by evaporation of the solvent from a mixture of metal-containing liquid crystalline (LC) mesophases of triblock copolymer and transition metal nitrate hydrate, and the carbon source is low-polymerized phenolic resol. Characterization by XRD, N(2) sorption isotherms, TEM, HRSEM, ICP-AES, TG, and XPS techniques has indicated an ordered 2D hexagonal mesostructure, high surface areas between 524 and 721 m(2) g(-1), uniform pore sizes of about 4.0 nm, large pore volumes ranging from 0.34 to 0.58 cm(3) g(-1), and metal contents ranging from 0.6 to 10.0 wt%. There is a high degree of dispersion, and a small size of nanoparticles throughout the whole framework, without aggregation outside of the pores due to the confinement effect of the mesoporous ordered matrix. The mesoporous solids show excellent adsorption properties for dyes and permit an easy magnetic separation procedure. This method is expected to be applicable to other mesoporous transition metal(oxide)-containing carbon catalysts. 相似文献
126.
Three lanthanide coordination polymers were prepared by hydrothermal synthesis and characterized by single-crystal X-ray diffraction. [Pr2(mBDC)3(phen)(H2O)]n·0.5nH2O (1) (mBDC=isophthalate, phen=1,10-phenanthroline) exhibits two kinds of metal environments (coordination numbers 7 and 8). In complex 1, mBDC ligands adopt the tetradentate (bridging and bridging) coordination mode and connect Pr ions into an undulating layer, and a 3D supramolecular structure is formed via hydrogen bonds between adjacent layers. [Tb4(mBDC)6(phen)]n (2) has three types of metal environments (coordination numbers 6, 7 and 8) and is composed of a 3D network formed by mBDC linking Tb ions via tetradentate (bridging and bridging) and pentadentate (bridging/chelating and bridging) coordination modes. There are two kinds of small quadrilateral channels along the a-axis. [Er4(mBDC)6(phen)]n (3) is isostructural to complex 2. 相似文献
127.
High-dimensional architectures from the self-assembly of lanthanide ions with benzenedicarboxylates and 1,10-phenanthroline 总被引:1,自引:0,他引:1
Six new coordination polymers, [Eu(1,2-BDC)(1,2-HBDC)(phen)(H(2)O)](n) (1), [Eu(2)(1,3-BDC)(3)(phen)(2)(H(2)O)(2)](n).4nH(2)O (2), [Eu(1,4-BDC)(3/2)(phen)(H(2)O)](n) (3), [Yb(2)(1,2-BDC)(3)(phen)(H(2)O)(2)](n).3.5nH(2)O (4), [Yb(2)(1,3-BDC)(3)(phen)(1/2)](n) (5), and [Yb(2)(1,4-BDC)(3)(phen)(2)(H(2)O)](n) (6), were synthesized by hydrothermal reactions of lanthanide chlorides with three isomers of benzenedicarboxylic acid (H(2)BDC) and 1,10-phenanthroline (phen), and characterized by single-crystal X-ray diffraction. 1 has a 2-D herringbone architecture with a Z-shaped cavity. 2 and 5 have different 3-D networks, but both are formed by 1,3-BDC anions bridging metal centers (Eu or Yb) via carboxylate groups. 3 and 6 possess similar layer structures which are further constructed to form 3-D networks by hydrogen bonds and/or pi-pi aromatic interactions. 4 comprises 1-D chains that are further interlinked via hydrogen bonds, resulting in a 3-D network. In the three europium complexes, all the europium ions are eight-coordinated, while the coordination numbers of the ytterbium ions in other three-coordination polymers range from six to eight. Crystal data: for 1, monoclinic, space group P2(1)/c, with a = 12.565(6) A, b = 16.005(8) A, c = 12.891(6) A, beta = 102.173(8) degrees, and Z = 4; for 2, monoclinic, space group P2(1)/c, with a = 20.979(4) A, b = 11.5989(19) A, c = 20.810(3) A, beta = 110.391(3) degrees, and Z = 4; for 3, triclinic, space group P1, with a = 10.331(5) A, b = 10.887(5) A, c = 11.404(5) A, alpha = 107.660(7) degrees, beta = 91.787(7) degrees, gamma = 112.946(6) degrees, and Z = 2; for 4, triclinic, space group P1, with a = 11.517(5) A, b = 13.339(5) A, c = 13.595(6) A, alpha = 87.888(7) degrees, beta = 67.759(6) degrees, gamma = 68.070(6) degrees, and Z = 2; for 5, orthorhombic, space group C222(1), with a = 8.174(2) A, b = 24.497(7) A, c = 29.161(8) A, and Z = 8; for 6, triclinic, space group P1, with a = 10.349(3) A, b = 11.052(3) A, c = 19.431(6) A, alpha = 105.464(4) degrees, beta = 91.300(5) degrees, gamma = 93.655(5) degrees, and Z = 2. The magnetic properties of 1 and 4 were investigated. The photophysical properties of 1 were also studied. 相似文献
128.
Wan H Holmén AG Wang Y Lindberg W Englund M Någård MB Thompson RA 《Rapid communications in mass spectrometry : RCM》2003,17(23):2639-2648
A high-throughput pKa screening method based on pressure-assisted capillary electrophoresis (CE) and mass spectrometry (MS) is presented. Effects of buffer type and ionic strength on sensitivity and pKa values were investigated. Influence of dimethyl sulfoxide (DMSO) concentration present in the sample on effective mobility measurement was examined. A series of ten volatile buffers, covering a pH range from 2.5 to 10.5 with the same ionic strength, was employed. The application of volatile background electrolytes resulted in significant signal increase as compared with commonly used non-volatile phosphate buffers. In general, the CE/MS system provided a ten-fold higher sensitivity than conventional UV detection. The newly developed CE/MS method offers high-throughput capacity by pooling a number of compounds into a single sample. Simultaneous measurement of more than 50 compounds was readily achieved in less than 150 min. The measured pKa values are consistent with the published data obtained from the CE/UV method and are also in good agreement with data generated by other methods. Other advantages of using CE/MS for pKa screening are illustrated with typical examples, including poorly soluble compounds and non-UV-absorbing compounds. 相似文献
129.
Weishun Liu Lin Fang Yinbo Wan Jianfang Zhang Guisheng Deng Jianbo Wang 《Tetrahedron》2019,75(7):855-861
In AgSbF6/Rh2(OAc)4/DCE system, two-component diastereoselective reactions of 2-diazo-3,5-dioxo-6-ynoates (phosphonates and sulphones) and alkenes provided easy access to 2-cyclopropyl-γ-pyrones through 6-endo-dig cyclization-cyclopropanation. In AgOAc/Rh2(OAc)4/Et3N/DCE system, two-component reaction of 2-diazo-3,5-dioxo-7-aryl-6-ynoates and alkenes afforded 2-cyclopropyl-2-alkylene-3(2H)-furanones through 5-exo-dig cyclization-cyclopropanation. The possible mechanism of reaction is discussed. A simple procedure and mild conditions are significant features of this strategy. 相似文献
130.
An efficient solution-processable route employing Pb(Ac)2 as lead source and anti-solvent treatment to achieve fully covered and homogenous perovskite films is reported. 相似文献