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Analysis of amino acids as their tert.-butyldimethylsilyl derivatives by gas-liquid chromatography and mass spectrometry 总被引:8,自引:0,他引:8
A gas-liquid chromatographic procedure is described which will separate and quantitate the seventeen amino acids typically found in protein acid hydrolyzates. If present, tryptophan, cysteine and carboxymethylcysteine can also be simultaneously assayed via this method. The amino acids, as their tert.-butyldimethylsilylated derivatives, are readily separable on SE-30 (wall-coated open-tubular) and OV-17 (bonded) capillary columns, as well as on packed gas-liquid chromatographic columns coated with the same liquid phases. Retention times and responses for all amino acids and internal standards are given. Mass spectral analysis of all tert.-butyldimethylsilylated amino acids is presented and displays a characteristic and unique [M- 57] fragment ion for each amino acid which often dominates the mass spectrum. Application of this method is demonstrated using four well characterized proteins. 相似文献
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Valeri V. Mossine Charles L. Barnes Thomas P. Mawhinney 《Journal of carbohydrate chemistry》2013,32(5):245-263
D-Fructosamine derivatives are key intermediates of the early Maillard reaction and have been a subject of numerous studies in food and health sciences due to their implication in the nutritional and organoleptic quality of foods, as well as to complications in diabetes and renal disease. We report the crystal structure analyses of 1-deoxy-β -D-fructopyranos-1-ylamine hydrochloride (1) and -hydroacetate (2) salts. The carbohydrate rings adopt the normal 2C5 pyranose chair conformation in 1 and 2. Bond lengths and valence angles in 1 and 2 compare well with the average values from related pyranose structures. There are two conformationally nonequivalent molecules in the asymmetric unit in 1. All hydroxyl and ring oxygen atoms, ammonium groups, and chloride ions in 1 are involved in an extensive three-dimensional hydrogen bonding network. The hydrogen bonding network in 2 is formed by one type of infinite chain with attached antidromic cycles. 相似文献
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Pisarenko AN Young R Quiñones O Vanderford BJ Mawhinney DB 《Inorganic chemistry》2011,50(18):8691-8693
Historically, the synthesis of perbromate ion through conventional oxidation routes has proven elusive. Herein, we report perbromate ion formation through the reaction of hypobromite and bromate ions in an alkaline sodium hypobromite solution. Formation was established via LC-MS/MS analysis of the bromate and perbromate ions in the reaction solutions over a 13-day period. Furthermore, it was discovered that the perbromate ion was also formed as a result of the electrospray ionization process. Selective reduction of the bromate ion prior to analysis was used to confirm the two formation pathways. 相似文献
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Kevin Lefrancois-Gagnon Robert Mawhinney 《International journal of quantum chemistry》2024,124(7):e27364
The properties of substituents have long been quantified by their effect elsewhere in a molecule. Ideally, intrinsic properties detailing the true properties of a substituent would be used. These properties are ideally transferable between molecules, to be robust and applied in different situations. Through a study on the bond critical point (BCP) properties of 117 substituents and 17 substrates we find that BCP properties from the quantum theory of atoms in molecules are not transferable between different bonded atoms. However, a substituent's changing electronegativity between substrates help quantify the observed variation. The relationship between changing electronegativities and critical point properties enables development of a relationship to predict critical point properties between a substituent and a new substrate, using only the electronegativity of a substituent attached to hydrogen, and the critical point property between the substituent and H. 相似文献
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M. Cheng S. Datta A. Francis J. van der Heide C. Jung O. Kaczmarek F. Karsch E. Laermann R. D. Mawhinney C. Miao S. Mukherjee P. Petreczky J. Rantaharju C. Schmidt W. Söldner 《The European Physical Journal C - Particles and Fields》2011,71(2):1-13
We present results for screening masses of mesons built from light and strange quarks in the temperature range of approximately between 140 MeV to 800 MeV. The lattice computations were performed with 2+1 dynamical light and strange flavors of improved (p4) staggered fermions along a line of constant physics defined by a pion mass of about 220 MeV and a kaon mass of 500 MeV. The lattices had temporal extents N τ =4, 6 and 8 and aspect ratios of N s /N τ ≥4. At least up to a temperature of 140 MeV the pseudo-scalar screening mass remains almost equal to the corresponding zero temperature pseudo-scalar (pole) mass. At temperatures around 3T c (T c being the transition temperature) the continuum extrapolated pseudo-scalar screening mass approaches very close to the free continuum result of 2πT from below. On the other hand, at high temperatures the vector screening mass turns out to be larger than the free continuum value of 2πT. The pseudo-scalar and the vector screening masses do not become degenerate even for a temperature as high as 4T c . Using these mesonic spatial correlation functions we have also investigated the restoration of chiral symmetry and the effective restoration of the axial symmetry. We have found that the vector and the axial-vector screening correlators become degenerate, indicating chiral symmetry restoration, at a temperature which is consistent with the QCD transition temperature obtained in previous studies. On the other hand, the pseudo-scalar and the scalar screening correlators become degenerate only at temperatures larger than 1.3T c , indicating that the effective restoration of the axial symmetry takes place at a temperature larger than the QCD transition temperature. 相似文献
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Antonio DJ Boyle PA Blum T Christ NH Cohen SD Dawson C Izubuchi T Kenway RD Jung C Li S Lin MF Mawhinney RD Noaki J Ohta S Pendleton BJ Scholz EE Soni A Tweedie RJ Yamaguchi A;RBC UKQCD Collaborations 《Physical review letters》2008,100(3):032001
We present the first results for neutral-kaon mixing using (2+1)-flavors of domain-wall fermions. A new approach is used to extrapolate to the physical up and down quark masses from our numerical studies with pion masses in the range 240-420 MeV; only SU(2)_{L}xSU(2)_{R} chiral symmetry is assumed and the kaon is not assumed to be light. Our main result is B_{K};{MS[over ]}(2 GeV)=0.524(10)(28) where the first error is statistical and the second incorporates estimates for all systematic errors. 相似文献
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Structural Chemistry - Tetracyanodiphenoquinodimethane (TCNDQ) and tetracyanopyrenoquinodimethane (TCNP) are larger cyanocarbons related to tetracyanoethylene (TCNE) and tetracyanoquinodimethane... 相似文献