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121.
122.
Methotrexate (MTX) has been convalently attached to an IgG-type monoclonal antibody (791T/36) directed to tumour-associated antigen gp72. Conjugates were synthesized by the active ester method using MTX N-succinimidyl ester at various pH values (7.5-10.5). Following purification by gel filtration, high performance liquid chromatography was used to assess the free drug or its derivatives in samples of MTX-791T/36 conjugates previously treated (or not) with hydroxylamine. Quantitative analysis, performed on a reversed phase column (pore size 300 A) with isocratic acetonitrile-sodium acetate buffer (pH 4.8) as mobile phase, indicated no detectable amount of free methotrexate in hydroxylamine-treated conjugates even six months after their preparation. Similar observations were made with conjugates, whose synthesis were performed at pH greater than or equal to 10. In contrast, the presence of increasing amounts of drug/metabolite could be demonstrated in samples produced at lower pH values. Based on these findings, the pH-dependent kinetics of MTX release has been determined and used to design conditions under which stable MTX-791T/36 conjugates could be prepared without hydroxylamine reaction.  相似文献   
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Sulfonic cation exchangers with two ion exchange group concentrations (0.5 and 2.4 mmol/g, samples A and B, respectively) were obtained by sulfonation of a porous styrene (S) and divinylbenzene (DVB) copolymer with chlorosulfonic acid. Strong thermal decomposition of the sulfonated copolymer A, accompanied by significant changes in its porous structure, starts at ca. 400°C. The char has no sulfonic groups. After heat treatment at 400°C in steam, a sorbent was obtained (yield 65%) that shows higher phenol sorption than the untreated sample when related to the bed volume. The chlorosulfonic derivatives of the initial copolymer were less thermally resistant than the sulfonic ones obtained by hydrolysis. Pyrolysis of the cation exchanger B, in its H+ and Ca2+ forms, was carried out at 900°C (yield of both chars close to 30%). By subsequent steam activation at 800°C to a 50% burn-off of the char, sorbents with well-developed, but distinctly different, porous structures were obtained. The activated char from the sulfonated copolymer in its hydrogen form was highly microporous and indicated an effective surface area of 1180 m2/g. However, because of a low contribution of mesopores, its ability to adsorb phenol from the liquid phase was not very high. The activated char from the calcium-doped copolymer, indicating a smaller surface area (580 m2/g) but characterized by a well-developed mesoporosity, was a better sorbent for phenol. © 1994 John Wiley & Sons, Inc.  相似文献   
125.
The centrosymmetric structure of {Cd[S2CN(CH2Ph)2]2}2 features both bridging and chelating dithiocarbamate ligands so that a square pyramidal S5 coordination geometry results. Copyright © 2004 John Wiley & Sons, Ltd.  相似文献   
126.
 A validation procedure based on the ISO/IEC 17025 standard was used to demonstrate the long-term stability of a calibration process and to assess the measurement uncertainty of a standard test method for optical emission vacuum spectrometric analysis of carbon and low-alloy steel (ASTM E 415–99a). The validation was used to provide documented evidence that the selected method fulfils the requirements and that the method is ”fit for purpose”. A test for drift was applied to determine statistically whether the analytical results vary systematically with time. The accuracy and traceability of the optimised method were tested by an analysis of closely matched matrix certified reference materials (CRMs). The measurement uncertainty estimations took account of the precision study, the bias and its uncertainty, and the qualification of uncertainties not considered in the overall performance studies. Received: 2 November 2002 Accepted: 2 January 2003 Acknowledgement The author expresses gratitude to Dr. Aleš Fajgelj for helpful discussions during the 3rd Central European Conference on Reference Materials and Measurements. Presented at CERMM-3, Central European Reference Materials and Measurements Conference: The function of reference materials in the measurement process, May 30–June 1, 2002, Rogaška Slatina, Slovenia Correspondence to T. Drglin  相似文献   
127.
Composites were prepared from an aerosil and 4-n-alkyl-4'cyanobiphenyls with five to eight carbon atoms in the alkyl chain. Their high silica density of ∼7 g aerosil in 1 cm3 of liquid crystal (LC) allows the observation of the behaviour of a thin cyanobiphenyl layer (having nearly a monolayer structure) on the silica particles. The systems are investigated by dielectric spectroscopy (10-2-109 Hz) in a large temperature range (220-370 K). All the composites show a (main) relaxation process at frequencies much lower than the processes observed for the bulk LC that was assigned to the dynamics of the molecules in the surface layer. The temperature dependence of its characteristic frequencies obeys the Vogel-Fulcher-Tammann law, which is found to be typical for glass-forming liquids. The quasi two-dimensional character of the glass transition in the surface layer is discussed for the first time. At the nematic-to-isotropic transition temperature of the bulk, the composites show a continuous decrease of the characteristic frequencies as a function of the alkyl chain length, while the bulk LCs show the well known odd-even behaviour. The magnitude and temperature dependence of the slow relaxation process in the composites (molecules on an outer surface) agree with those of the same molecules confined to the nanopores of molecular sieves (internal surface).  相似文献   
128.
The quantitative and kinetic parameters of sorption of formic and acetic acids on thin films of various modifiers of piezoelectric quartz resonator electrodes are determined. Parameters of film formation on the electrodes (application procedure and thickness) are optimized. Methods for joint and separate determination of formic and acetic acids in air by piezoelectric microweighing with single- and double-sensor devices are developed.  相似文献   
129.
The reactivity of square planar palladium(II) and platinum(II) complexes in trans or cis configuration, namely trans or cis‐[dichlorobis(tributylphosphine)platinum(II)] and trans‐[dichlorobis(tributylphosphine)palladium(II)] with 1,1′‐bis(ethynyl) 4,4′‐biphenyl, DEBP, leading to π‐conjugated organometallic oligomeric and polymeric metallaynes, was investigated by a systematic variation of the reaction conditions. The formation of polymers and oligomers with defined chain length [? M(PBu3)2 (C?C? C6H4? C6H4? C?C? )]n (n = 3–10 for the oligomers, n = 20–50 for the polymers) depends on the configuration of the precursor Pt(II) and Pd(II) complexes, the presence/absence of the catalyst CuI, and the reaction time. A series of model reactions monitored by XPS, GPC, and NMR 31P spectroscopy showed the route to modulate the chain growth. As expected, the nature of the transition metal (Pt or Pd) and the molecular weight of the polymers markedly influence the photophysical characteristics of the polymetallaynes, such as optical absorption and emission behavior. Polymetallaynes with nanostructured morphology could be obtained by a simple casting procedure of polymer solutions. © 2007 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 45: 3311–3329, 2007  相似文献   
130.
Normal silica glass is usually referred to as low density amorphous silica as it can be converted to high density amorphous silica by a hydrostatic pressure (polyamorphic transition). In this work in situ Raman experiments are performed in a diamond anvil cell up to 18 GPa. The pressure effects on the structure of silica after successive compression decompression experiments are analyzed. The mode Grüneisen parameters corresponding to the elastic compression of high density amorphous silica are obtained and compared with those of normal silica. A reorganization of the high density amorphous silica below 3 GPa is evidenced.  相似文献   
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