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141.
A capillary zone electrophoresis-negative electrospray ionization-quadrupole time of flight-mass spectrometric method was developed for the characterization of oligonucleotides after synthesis, using model compounds. The major difficulty is the adduction of metal cations to the polyanionic backbone of the oligonucleotide sample, resulting in complex spectra and decreased sensitivity. Several approaches were investigated to circumvent this problem. Separation was performed in an ammonium carbonate buffer. During separation, the interfering metal ions were exchanged for ammonium ions, which are less tightly bound to the oligonucleotide when ionized. The influence of the addition of piperidine and imidazole or trans-1,2-diaminocyclohexane-N,N,N',N'-tetraacetic acid (CDTA) to the running buffer for further reduction of cation adduction was investigated. Addition of CDTA to the buffer system resulted in a deconvoluted spectrum with very little adducts. On-line sample stacking proved vital to preconcentrate the samples. The pH and the concentration of the ammonium carbonate buffer as well as the electrophoresis voltage were optimized to achieve the best signal response for the oligonucleotides and a maximum reduction of the cation adducts as well as a short analysis time. Finally, the sheath liquid composition was examined for further improvement of the signal. The developed method was used to analyze different oligonucleotides (5000-9200 Da) in light of its use as a final quality control method for oligonucleotides in terms of purity and sequence homogeneity of the synthesized products. In all cases, very little adducts were observed in the deconvoluted spectra, and the relative errors of the measured molecular masses ranged from 3 to 35 ppm. 相似文献
142.
A novel three-dimensional metal selenite [Fe2(H2O)4(SeO3)2] (1) has been hydrothermally synthesized and characterized by the elemental analyses, IR spectrum, TG analysis and the single crystal X-ray diffraction. Compound 1 crystallizes in the monoclinic system, space group P21/n, with a=6.5283(13) Å, b=8.8754(18) Å, c=7.6798(15) Å, (=98.82(3)β, V=439.71(15) Å3, and Z=2. Compounds 1 exhibits interesting three-dimensional structure constructed from {FeO6} octahedra and {SeO3} pyramids linked via the corner- and/or edge-sharing mode. The most interesting structural feature of compound 1 is that the existence of multidirectional intersecting double helical chains in one compound. 相似文献
143.
A novel near infrared (NIR) modeling method—Laplacian regularized least squares regression (LapRLSR) was presented, which can take the advantage of many unlabeled spectra to promote the prediction performance of the model even if there are only few calibration samples. Using LapRLSR modeling, NIR spectral analysis was applied to the online monitoring of the concentration of salvia acid B in the column separation of Salvianolate. The results demonstrated that LapRLSR outperformed partial least squares (PLS) significantly, and NIR online analysis was applicable. 相似文献
144.
Yu-Dong Shen Hai-Qiang Wu Xian-Zhang Bu Lin-Kun An Pei-Qing Liu Yue-Ming Li 《Tetrahedron》2005,61(38):9097-9101
A novel procedure to construct o-naphthothiophenequinones has been achieved from readily available o-benzothiophenquinones and N-dienes via Diels-Alder reaction-aromatization sequence as key steps. The absolute regioselectivity was established via Diels-Alder reaction of o-benzothiophenquinones with rich electron N-dienes. 相似文献
145.
Optical Review - Based on the planar optical theory, compact beam expanders are proposed to miniaturize the dimension of an optical system. Both simulated and experimental results have demonstrated... 相似文献
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148.
Wenyu Zhao Shengli An Bin Fan Songbo Li 《Applied Physics A: Materials Science & Processing》2014,116(3):987-991
Tm3+ and In3+ co-doped LaAlO3 phosphors were prepared by a Pechini sol–gel method and characterized by X-ray diffraction, scanning electron microscope, and cathodoluminescence spectrum. The phosphor is composed of slightly aggregated particles with approximately spherical shape and a narrow size range of 1.0–1.5 μm. Under voltage electron beam excitation, the phosphor shows the characteristic emissions of Tm3+. All the color purity, radiant efficiency, luminous efficiency, and stability of the optimum LaAlO3:0.01Tm3+, 0.04In3+ phosphor are superior to these of commercial ZnS:Ag,Cl phosphor. These tests suggest that it could be a potential candidate as a blue phosphor for field emission displays. 相似文献
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Damla Durak Anıl Delikanlı Cahit Demetgül İbrahim Kani Selahattin Serin 《Transition Metal Chemistry》2013,38(2):199-206
An unsymmetrical tetradentate Schiff base (H2L) was synthesized by the reaction of 3-methoxysalicylaldehyde, o-phenylenediamine, and salicylaldehyde in EtOH. H2L was characterized by single-crystallographic X-ray analysis. Its Co(II) and Mn(III) complexes ([CoL] and [MnLCl]) were prepared and immobilized on 3-aminopropyltriethoxysilane functionalized silica gel. The immobilized materials were found to be efficient catalysts for epoxidation of styrene in the presence of tert-BuOOH in acetonitrile at 40 °C. The catalysts can be reused several times without significant loss of performance. 相似文献