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Explanation through density functional theory of the unanticipated loss of CO2 and differences in mass fragmentation profiles of ritonavir and its rCYP3A4‐mediated metabolites 下载免费PDF全文
Shalu Jhajra Tarun Handa Sonam Bhatia P. V. Bharatam Saranjit Singh 《Journal of mass spectrometry : JMS》2014,49(6):452-467
In the present study, the metabolism of ritonavir was explored in the presence of rCYP3A4 using a well‐established strategy involving liquid chromatography–mass spectrometry (LC–MS) tools. A total of six metabolites were formed, of which two were new, not reported earlier as CYP3A4‐mediated metabolites. During LC–MS studies, ritonavir was found to fragment through six principal pathways, many of which involved neutral loss of CO2, as indicated through 44‐Da difference between masses of the precursors and the product ions. This was unusual as the drug and the precursors were devoid of a terminal carboxylic acid group. Apart from the neutral loss of CO2, marked differences were also observed among the fragmentation pathways of the drug and its metabolites having intact N‐methyl moiety as compared to those lacking N‐methyl moiety. These unusual fragmentation behaviours were successfully explained through energy distribution profiles by application of the density functional theory. Copyright © 2014 John Wiley & Sons, Ltd. 相似文献
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Jaspreet S. Dhau Amritpal Singh Yoganjaneyulu Kasetti Sonam Bhatia Parsad V. Bharatam Paula Brandão Vítor Félix Kamal N. Singh 《Tetrahedron》2013
The BF3-directed lithiation of 3-chloro- and 3-bromopyridine (1a and 1b, respectively) has been investigated. The reactions of 3-chloro- or 3-bromopyridine–BF3 adduct with LDA (1.3/1.1 equiv) followed by quenching with benzaldehyde or iodine exclusively gave the C-2 substituted products. However, when 2.2 equiv of LDA and dimethyl disulfide was used, a C-6 substituted product was obtained. Dilithiation of 1a and 1b has been studied with and without the involvement of BF3 complexation. The role of Li?F(BF3) interactions has been investigated by experimental and DFT calculations. 相似文献
205.
N. M. Bhatia P. A. Pathade H. N. More P. B. Choudhari S. D. Jadhav M. S. Bhatia 《Journal of Analytical Chemistry》2013,68(10):924-930
Verapamil is a calcium channel blocking agent which has found widespread use in the management of supraventricular tachyarrhythmias, angina pectoris, hypertrophic cardiomyopathy and hypertension. It is converted to its biologically active metabolite nor-verapamil in liver by cytochrome P450. In present communication, synthesis and characterization of nor-verapamil and development of reverse phase high performance liquid chromatographic method for the quantification of nor-verapamil along with verapamil in plasma has been carried out. The characterization of nor-verapamil was carried out using GC-MS, FT-IR and NMR spectroscopy. The separation was carried out with an isocratic JASCO RP-HPLC system using 5 μm KYA TECH HiQ Sil C18 HS column (250 mm × 4.6 mm internal diameter) as a stationary phase and methanol: water: 0.01 M orthophosphoric acid: triethylamine [70: 30: 2: 0.5, v/v/v/v] as mobile phase. The flow rate was maintained at 1.0 mL/min and UV detection at 222 nm. The calibration for verapamil and nor-verapamil were found to be linear over concentration range of 50–300 ng/mL with correlation coefficient (n = 6) of 0.9995 and 0.9997, respectively. This method was validated according to USFDA guidelines. The method was found to be simple, accuare, precise sensitive and selective for the determination of verapamil and nor-verapamil in plasma and thus useful in bioequivalence studies of verapamil. 相似文献
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Hossein A. Baghdadi Heidi Sardinha Surita R. Bhatia 《Journal of Polymer Science.Polymer Physics》2005,43(2):233-240
We report results on the rheology of a model polymer/clay system, laponite clay particles with added poly(ethylene oxide) (PEO), focusing on the kinetics of gel formation and on molecular weight effects. We examined solutions at both pH = 7, where interparticle attractions are present and a networked gel is formed; and at pH = 10, where repulsive forces dominate and laponite forms a colloidal glass. We found that PEO of low to moderate molecular weight significantly slows down gelation and decreases the complex viscosity and elastic modulus of the dispersion by several orders of magnitude for both pH = 7 and 10. In the former case, adsorbed PEO likely forms a steric barrier to the formation of an attractive gel. In the latter case, we propose that free PEO chains in solution induce a depletion attraction between particles, preventing or slowing the formation of a colloidal glass. At higher molecular weights, PEO chains are long enough to bridge between particles and form an associative network, enhancing the viscosity and elastic modulus for both pH = 7 and 10. Finally, we have shown the critical molecular weight for transitioning between these two types of behavior scales with the interparticle distance. © 2004 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 43: 233–240, 2005 相似文献
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Mahender Singh K. L. Bhatia N. Kishore Partap Singh R. S. Kundu 《Journal of Non》1995,180(2-3):251-259
AC conductivity and dielectric relaxation measurements of the bulk amorphous compositions in the pseudo-binary system (As2S3)1-x(PbS)x (x = 0, 0.1, 0.4 and 0.5) in the frequency range 500 Hz-10 kHz and in the temperature span 180–450 K are reported. The temperature dependence of the ac conductivity, σac(ω), has a broad structure at all frequencies in compositions with x = 0.1, 0.4 and 0.5 whose peak position is not thermally activated. A similar structure was also observed in the data on the dielectric constant, ε1, which peaked at a frequency of 1 kHz in the composition with x = 0.5. Analysis of the results using the correlated barrier hopping model revealed that the electronic conduction takes place by single polaron and bipolaron hopping processes at high and low temperatures, respectively, in compositions containing Pb. The microstructure and phase-separation in the glasses containing Pb influence the electrical transport and dielectric dispersion. This study has revealed the possible presence of a phase transformation at around 300 K at a frequency of 1 kHz in the dielectric dispersion behaviour of composition with x = 0.5. 相似文献
209.
Inequalities that compare unitarily invariant norms of A - B and those of AΓ - ΓB and Γ-1A - B Γ-1 are obtained, where both A and B are either Hermitian or unitary or normal operators and Γ is a positive definite operator in a complex separable Hilbert space. These inequalities are then applied to derive bounds for spectral variation of diagonalisable matrices. Our new bounds improve substantially previously published bounds. 相似文献
210.
We provide a new approach to Lidskii’s theorem relating the eigenvalues of the differenceA—B of two self-adjoint matrices to the eigenvalues ofA andB respectively. This approach combines our earlier work on the spectral matching of matrices joined by a normal path with some
familiar techniques of functional analysis. It is based, therefore, on general principles and has the additional advantage
of extending Lidskii’s result to certain pairs of normal matrices. We are also able to treat some related results on spectral
variation stemming from the work of Sunder, Halmos and Bouldin. 相似文献