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41.
Because of the potential in-source conversion between a lactone and the corresponding hydroxy acid, it has been recognized that a liquid chromatography/tandem mass spectrometric (LC/MS/MS) method developed for quantitation of a lactone drug in the presence of its hydroxy acid metabolite (or vice versa) must incorporate chromatographic separation between the two compounds, unless in-source conversion between the two compounds has been eliminated by the appropriate selection of the LC/MS/MS parameters. We now report that chromatographic separation between a lactone and its hydroxy acid will be required under certain LC/MS/MS conditions used even in the absence of in-source conversion. This is due to the fact that the 18-mass-unit difference between a lactone and its hydroxy acid is, by coincidence, different by only one mass unit from the 17-mass-unit difference between the [M + H](+) and [M + NH(4)](+) ions of the lactone or the hydroxy acid. Thus, the [M + H](+) ion of a hydroxy acid is higher than the [M + NH(4)](+) ion of its lactone by only one mass unit. Therefore, in a method developed for quantitation of a hydroxy acid drug utilizing a selected-ion-monitoring (SRM) scheme that incorporates its [M + H](+) ion as the precursor ion, the quantitation would be inaccurate due to the interference by the contribution of the A + 1 isotope response from the [M + NH(4)](+) ion of the lactone metabolite present in the sample, unless there is a chromatographic separation between the two compounds. This is true even if Q1 is operated under a unit-mass resolution. The implication of this type of interference, arising from the presence of both the [M + H](+) and [M + NH(4)](+) ions of a drug and its metabolite, to the selection of LC and MS conditions (including mass resolution) will be discussed using the data obtained with a model lactone drug and its hydroxy acid metabolite. 相似文献
42.
Sonia Jebri Ali Bechrifa Mohamed Jemal 《Journal of Thermal Analysis and Calorimetry》2012,109(2):1059-1067
Phosphobaryum carbonate hydroxyapatites Ba10(PO4)6(OH)(2?2x)(CO3) x with 0????x????1, were synthesized in this study by solid gas reaction at a high temperature. Carbonate content was determined by thermogravimetric analysis and X-ray diffraction. The heat of the solution in a 3 wt% nitric acid solution was measured at 298?K using an isoperibol calorimeter. The combination of the enthalpies of solution with the enthalpies of formation of the reactants allowed us to determine the standard enthalpies of formation of the studied apatites. The result showed a decrease in formation enthalpy with the carbonate amount introduced in the lattice, suggesting an increase in stability of these compounds as the ratio of the substitution increases. 相似文献
43.
Commercial disodium hydrogen phosphate dodecahydrate (Na2HPO4·12H2O) was used as a precursor for synthesizing disodium hydrogen phosphate hexahydrate (Na2HPO4·6H2O) and sodium diphosphate (Na4P2O7). The purity of the synthesized products was checked up by IR spectroscopy and X-ray diffraction. The heat of dissolution of these compounds, in acid solutions of several concentrations (w/w) of H3PO4 was measured in a C-80 SETARAM calorimeter. Many dilution and mixing processes were also realized in the calorimeter in order to get the standard enthalpy of formation of these products. The values obtained for the enthalpies of formation are: (?3210.5) and (?3516.5) kJ · mol?1 for sodium diphosphate (Na4P2O7) and disodium hydrogen phosphate hexahydrate (Na2HPO4·6H2O), respectively. 相似文献
44.
Recently, we have developed liquid chromatography/tandem mass spectrometry (LC/MS/MS)-based methods for the quantitation of pegylated therapeutic proteins in plasma. The methods are based on the LC/MS/MS detection of a surrogate peptide generated from trypsin digestion of the therapeutic protein. Various parameters related to the bioanalytical methods were evaluated and optimized, including the preparation of calibration standards and quality control samples, sample extraction, internal standard selection and its stage of addition, trypsin digestion, and non-specific binding. In this paper, we report the development of a method for a specific pegylated therapeutic protein and detail the various optimization steps undertaken. Simple extraction of the pegylated therapeutic protein from plasma was achieved via the precipitation of the endogenous proteins in plasma using acidic isopropanol and the resulting supernatant extract was subjected to trypsin digestion. A unique tryptic peptide arising from the pegylated therapeutic protein was used for LC/MS/MS-based detection and quantitation. A protein and a peptide were used as internal standards, with the former added before the sample extraction and the latter after the sample extraction. The method developed is simple, sensitive, specific and rugged, and has been implemented in a high throughput 96-well format to analyze plasma samples from in vivo studies. A required lower limit of quantitation (LLOQ) of 10 ng/mL, expressed in terms of the concentration of the protein drug, was easily achieved. 相似文献
45.
Jemal Yimer Damte Zhan-Jun Zhu Pin-Jun Lin Chen-Hao Yeh Jyh-Chiang Jiang 《Journal of computational chemistry》2020,41(3):194-202
Methane conversion by using transition metal catalysts plays in an important role in various usages of the industrial process. The mechanism of methane conversion on B, N-co-doped graphene supported Ir and Pt clusters, BNG-Ir4 and BNG-Pt4, have been investigated using density functional theory calculations. Methane was found to adsorb on BNG-Ir4 and BNG-Pt4 clusters via strong agostic interactions. The first step of methane dehydrogenation on BNG-Ir4 has a lower energy barrier, indicating a facile methane dissociation on BNG-Ir4. In addition, it shows that hydrogen molecule can form on the BNG-Ir4 and hydrogen can desorb from the surface. Besides, the C-C coupling reaction of CH3 to form ethane is a more thermodynamically favorable process than CH3 dehydrogenation on BNG-Ir4. Further, ethane is easier to desorb from the surface due to its low desorption energy. Therefore, the BNG-Ir4 cluster is a potential catalyst for activating methane to form ethane and to produce hydrogen. © 2019 Wiley Periodicals, Inc. 相似文献
46.
A growing or shrinking disc will adopt a conical shape, its intrinsic geometry characterized by a surplus angle phi(e) at the apex. If growth is slow, the cone will find its equilibrium. Whereas this is trivial if phi(e)0. We construct these states in the regime where bending dominates and determine their energies and how stress is distributed in them. For each state a critical value of phi(e) is identified beyond which the cone touches itself. Before this occurs, all states are stable; the ground state has twofold symmetry. 相似文献
47.
48.
Hellali D. Zamali H. Sebaoun A. Jemal M. 《Journal of Thermal Analysis and Calorimetry》1999,57(2):569-574
The phase diagram of the binary AgNO3–CsNO3 system was constructed using differential thermal analysis (DTA) technique in the range 300–700 K. The apparatus is described briefly. The results exhibit a congruently melting compound CsNO3·AgNO3 (m.p.=453 K) characterized by two allotropic varieties and , an incongruently melting compound AgNO3·CsNO3 (m.p.=450 K) with three forms , and , two eutectics (16 mol% CsNO3, 442 K and 32.5 mol% CsNO3, 445 K) and a peritectic (38mol% CsNO3, 450 K). The occurrence of the transitions of intermediates was confirmed by X-ray diffraction at variable temperatures. The phase diagram exhibits also two plateaus at 429 K and 435 K corresponding to the phase transitions of CsNO3 and AgNO3, respectively.This revised version was published online in November 2005 with corrections to the Cover Date. 相似文献
49.
50.
Furlong MT Ouyang Z Wu S Tamura J Olah T Tymiak A Jemal M 《Biomedical chromatography : BMC》2012,26(8):1024-1032
For the development of human antibody Fc (fraction crystallizable) region-containing therapeutic protein candidates, which can be either monoclonal antibodies (mAbs) or pharmacologically active proteins/peptides fused to the Fc region of human Immunoglobulin G (IgG), reliable quantification of these proteins in animal pharmacokinetic study plasma samples is critical. LC-MS/MS has emerged as a promising assay platform for this purpose. LC-MS/MS assays used for bioanalysis of human antibody Fc region-containing therapeutic protein candidates frequently rely upon quantification of a 'signature' surrogate peptide whose sequence is unique to the protein analyte of interest. One drawback of the signature peptide approach is that a new LC-MS/MS assay must be developed for each new human Fc region-containing therapeutic protein. To address this issue, we propose an alternative 'universal surrogate peptide' approach for the quantification of human antibody Fc region-containing therapeutic protein candidates in plasma samples from all nonclinical species. A single surrogate tryptic peptide was identified in the Fc region of most human antibody Fc-containing therapeutic protein candidates. An LC-MS-MS method based upon this peptide was shown to be capable of supporting bioanalysis of a diversity of human Fc region-containing therapeutic protein candidates in plasma samples of all commonly used animal species. 相似文献