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991.
Temperature-gradient gel electrophoresis (TGGE) is a technique for studying the structural transitions of nucleic acids and proteins. A temperature gradient is formed in a horizontal slab gel perpendicular to the direction of the electric field. Whereas the principle of the TGGE method has previously been applied to proteins, we describe in this report the systematic optimization of TGGE as a routine technique for the quantitative analysis of conformational transitions in proteins. Using alpha-amylase as an example we show the kinds of results which may be obtained from such measurements. Buffers suitable for use in gel electrophoresis were analyzed with respect to the dependence of their pH value upon temperature. The correct pH range for TGGE of a given protein is determined by electrophoretic titration curves. The protein bands are detected by silver and/or activity staining. The thermal denaturation of alpha-amylase from Aspergillus oryzae showed a discontinuous transition into the denatured conformation, which exhibited much slower electrophoretic mobility. The discontinuity is due to an irreversible denaturation process under the gel conditions. The transition temperature was measured as a function of several parameters, e.g., the concentration of Ca(+)+, dithiotreithol, urea and the pH value. The structural transition of alpha-amylase is accompanied by a loss of enzymatic activity as determined by activity staining or by an activity assay carried out in solution. The structural transitions of two other alpha-amylases from Bacillus subtilis and Bacillus licheniformis were also studied. The results show that the TGGE method is simple to perform and allows the analysis of conformational transitions of proteins in a wide variety of conditions.(ABSTRACT TRUNCATED AT 250 WORDS) 相似文献
992.
Peter Sieber Bruno Kamber Albert Hartmann Albert Jhl Bernhard Riniker Werner Rittel 《Helvetica chimica acta》1974,57(8):2617-2621
A preliminary account is given of a total synthesis of human insulin involving directed formation of the three disulfide bonds at different stages of the fragment-condensation approach. The synthesis was facilitated by the application of two new methods for the selective removal of protecting groups. In the first, two S-Trt-protected cysteine residues are converted to the disulfide without affecting S-Acm-protected cysteine residues. The second new method consists in a very mild, pH-controlled, acidolysis of N(α)-Trt, leaving intact N(α)-Bpoc and other acid-labile protecting groups. The last step of the synthesis was the formation of the disulfide bridge between the Acm-protected cysteine residues A7 and B7 by iodine. Extensive counter-current distribution yielded the synthetic hormone in pure form. It was compared and found to be identical with natural human insulin. Identification was achieved by means of thinlayer chromatography and electrophoretic procedures, as well as by comparing the pattern of break-down by enzymes (finger-printing). The natural and synthetic hormones were crystallized under identical conditions. The synthetic human insulin was found to possess full biological activity in an in vitro system. 相似文献
993.
Bruno Bosbach 《Semigroup Forum》1976,12(1):119-135
In this paper we continue the study of Tbk-semigroups [1]. We define a weak Tbk-semigroup as an algebra (s,·,) which satisfies (A1) a(bc) = (ab)c, (A2) (S, ) is a semilattice, (A3) × (a b) y = xay xby, (A4) a (a b) S S (a b) . We shall prove that every weak Tbk-semigroup can be embedded into a Tbk-semigroup with 1, and we shall show that the theory of [1] can be developed already in weak Tbk-semigroups.
Über den Inhalt dieser Note berichtete der Autor verschiedene Male , zuletzt im Juni 1974 an der T.U. München. 相似文献
Über den Inhalt dieser Note berichtete der Autor verschiedene Male , zuletzt im Juni 1974 an der T.U. München. 相似文献
994.
Zheng Bo Jian Hua Yan Xiao Dong Li Yong Chi Bruno Chéron Ke Fa Cen 《Plasma Chemistry and Plasma Processing》2007,27(6):691-700
The dependence of gliding arc gas discharge characteristics, including gas flow field, arc column motion and volatile organic
compounds (VOCs) decomposition performance, on reactor configuration parameters was investigated based on numerical simulation
and laboratory experimental findings. For a given supply voltage (10 kV) and a certain nozzle outlet diameter (1.5 mm), increasing
the electrodes gap (1–4 mm) or decreasing vertical distance between electrode throat and nozzle outlet (25–10 mm) will increase
the gas flow rate through the electrode throat, the gas velocity in the plasma region, the arc column velocity, the maximum
attainable position of the arc column and the electrical power consumption, also, higher VOCs decomposition rate and lower
specific energy requirement are observed according to the n-butane and toluene decomposition experiments. 相似文献
995.
Bastiat G Grassl B Khoukh A François J 《Langmuir : the ACS journal of surfaces and colloids》2004,20(14):5759-5769
Sodium dodecyl sulfate (SDS)-poly(propylene oxide) methacrylate (PPOMA) (of molecular weight M(w) = 434 g x mol(-1)) mixtures have been studied using conductimetry, static light scattering, fluorescence spectroscopy, and 1H NMR. It has been shown that SDS and PPOMA form mixed micelles, and SDS and PPOMA aggregation numbers, N(ag SDS) and N(ag PPOMA), have been determined. Total aggregation numbers of the micelles (N(ag SDS) + N(ag PPOMA)) and those of SDS decrease upon increasing the weight ratio R = PPOMA/SDS. Localization of PPOMA inside the mixed micelles is considered (i) using 1H NMR to localize the methacrylate function at the hydrophobic core-water interface and (ii) by studying the SDS-PPO micellar system (whose M(w) = 400 g x mol(-1)). Both methods have indicated that the PPO chain of the macromonomer is localized at the SDS micelle surface. Models based on the theorical prediction of the critical micellar concentration of mixed micelles and structural model of swollen micelles are used to confirm the particular structure proposed for the SDS-PPOMA system, i.e., the micelle hydrophobic core is primarily composed of the C12 chains of the sodium dodecyl sulfate, the hydrophobic core-water interface is made up of the SDS polar heads as well as methacrylate functions of the PPOMA, the PPO chains of the macromonomer are adsorbed preferentially on the surface, i.e., on the polar heads of the SDS. 相似文献
996.
Carbon-13 NMR spin-lattice relaxation times (T1) were measured for morphine, oxymorphone, nalorphine, naloxone and naltrexone as hydrochloride salts in 2H2O solution. The data refer to the molecules in the N-equatorial configuration. The experimental T1 values were interpreted using a model of anisotropic reorientation of a rigid body with superimposed internal motions of the flexible N-methyl, N-methyl-allyl and N-methyl-cyclopropyl fragments. The calculated internal motional rates were found to markedly decrease on passing from agonists to mixed (nalorphine) and pure (naloxone, naltrexone) antagonists. For these latter the observed trend of the internal flexibility about N---C and C---C bonds of the N-substituents is discussed in terms of a correlation with their relative antagonistic potencies. In fact, such an evidence of decreasing internal conformational dynamics in the order nalorphine, naloxone, naltrexone, appeared interestingly in line with the “two-state” model of opiate receptor operation mode proposed by Snyder. 相似文献
997.
Analysis of BTEX, PAHs and metals in the oilfield produced water in the State of Sergipe, Brazil 总被引:2,自引:0,他引:2
Haroldo S. Drea Jos R.L. Bispo Kennedy A.S. Arago Bruno B. Cunha Sandro Navickiene Jos P.H. Alves Luciane P.C. Romo Carlos A.B. Garcia 《Microchemical Journal》2007,85(2):234-238
During oil and gas exploitation, large amounts of produced water are generated. This water has to be analyzed with relation to the chemical composition to deduce the environmental impact of its discharge after a treatment process. Therefore, a study was carried out to evaluate preliminarily the BTEX (benzene, toluene, ethylbenzene and xylenes), polycyclic aromatic hydrocarbons (PAHs) and metals contents in produced water samples taken from effluents of the Bonsucesso treatment plant located in the city of Carmópolis, the most important oil and gas producer in the State of Sergipe, North-east of Brazil. Three methods were optimized to determine the target compounds. Polycyclic aromatic hydrocarbons were determined by gas chromatography with mass spectrometric detection (GC/MS), volatile aromatic hydrocarbons (BTEX) by gas chromatography with photoionization detector (GC/PID) and metals were analyzed by flame atomic absorption spectrometry (FAAS). The results showed that concentrations of the target compounds in these samples ranged from 96.7 to 1397 μg L− 1 for BTEX, from 0.9 to 10.3 μg L− 1 for PAHs and from 0.003 to 4540 mg L− 1 for metals. 相似文献
998.
The implementation of quality systems in analytical laboratories has now, in general, been achieved. While this requirement significantly modified the way that the laboratories were run, it has also improved the quality of the results. The key idea is to use analytical procedures which produce results that fulfil the users needs and actually help when making decisions. This paper presents the implications of quality systems on the conception and development of an analytical procedure. It introduces the concept of the lifecycle of a method as a model that can be used to organize the selection, development, validation and routine application of a method. It underlines the importance of method validation, and presents a recent approach based on the accuracy profile to illustrate how validation must be fully integrated into the basic design of the method. Thanks to the -expectation tolerance interval introduced by Mee (Technometrics (1984) 26(3):251–253), it is possible to unambiguously demonstrate the fitness for purpose of a new method. Remembering that it is also a requirement for accredited laboratories to express the measurement uncertainty, the authors show that uncertainty can be easily related to the trueness and precision of the data collected when building the method accuracy profile. 相似文献
999.
Goudreau N Brochu C Cameron DR Duceppe JS Faucher AM Ferland JM Grand-Maître C Poirier M Simoneau B Tsantrizos YS 《The Journal of organic chemistry》2004,69(19):6185-6201
The virally encoded NS3 protease is essential to the life cycle of the hepatitis C virus (HCV), an important human pathogen causing chronic hepatitis, cirrhosis of the liver, and hepatocellular carcinoma. The design and synthesis of 15-membered ring beta-strand mimics which are capable of inhibiting the interactions between the HCV NS3 protease enzyme and its polyprotein substrate will be described. The binding interactions between a macrocyclic ligand and the enzyme were explored by NMR and molecular dynamics, and a model of the ligand/enzyme complex was developed. 相似文献
1000.
Le Bizec B Antignac JP Bertrand D Qannari el M Andre F 《Rapid communications in mass spectrometry : RCM》2005,19(4):509-518
The differentiation of stereoisomers on the basis of their mass spectra only is usually a difficult challenge even when an informative ionization technique such as electron ionization is used; this is particularly the case for steroids. In this study, multivariate statistical techniques have been applied to the mass spectra of derivatized 5xi-androstane-3xi,17xi-diols (xi = alpha,beta) in order to investigate the possibility of discrimination among the different isomers. After collection of the data from the mass spectra (20 replicates for each of the 8 isomers), each ion was considered as a statistical variable and each mass spectrum as an observation. The more discriminative variables (42 out of the 160 initial ones) were selected using the analysis of variance technique (ANOVA). Thereafter, a linear discriminant analysis (LDA) allowed us to set up a predictive model for stereochemistry determination. The two-dimensional graphical display of the 160 observations on the basis of the canonical variables derived from LDA made it possible to separate the eight isomers. The discrimination of 5alpha and 5beta isomers as well as 3alpha and 3beta was unambiguous, whereas, the discrimination of 17alpha and 17beta epimers was less obvious. The robustness of the model was checked with 40 mass spectra recorded over a 6-month period on different quadrupole mass spectrometers and under different signal acquisition conditions. The percentage of correct assignment of these 'unknown' stereoisomers was 92%; only three 17alpha and 17beta epimers were not correctly plotted in the expected zone. Nevertheless, the performance score was better than those observed with traditional mass spectral libraries. Furthermore, this statistical approach allowed us to identify the main fragment ions involved in the discrimination between isomers: m/z 256 and 421 for isomers 5a-5b; m/z 241 and 331 for isomers 5alpha3alpha-5alpha3beta; m/z 143 and 162 for isomers 5beta3alpha-5beta3beta; and m/z 255 for epimers 17alpha-17beta. 相似文献