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31.
A simple, sensitive and rapid assay method has been developed and validated as per regulatory guidelines for the estimation of enasidenib on mouse dried blood spots (DBS) using liquid chromatography coupled to tandem mass spectrometry with electrospray ionization in the positive‐ion mode. The method employs liquid extraction of enasidenib from DBS disks of mouse whole blood followed by chromatographic separation using 0.2% formic acid–acetonitrile (25:75, v/v) at a flow rate of 1.0 mL/min on an Atlantis dC18 column with a total run time of 2.0 min. The MS/MS ion transitions monitored were m/z 474.0 → 267.1 for enasidenib and m/z 309.2 → 251.3 for the internal standard (warfarin). The assay was linear in the range of 1.01 – 3044 ng/mL. The within‐run and between‐run precisions were in the range of 3.18 – 9.06 and 4.66 – 8.69%, respectively. Stability studies showed that enasidenib was stable on DBS cards for 1 month. This novel method has been applied to analyze the DBS samples of enasidenib obtained from a pharmacokinetic study in mice. 相似文献
32.
Saroha Rakesh Panwar Amrish K. Gaur Anurag Sharma Yogesh Kumar Vinay Tyagi Pawan K. 《Journal of Solid State Electrochemistry》2018,22(8):2507-2513
Journal of Solid State Electrochemistry - In the present work, olivine-layered composites, i.e., LiFePO4-Li2MnO3, are successfully synthesized in the form of a single monolithic electrode and layer... 相似文献
33.
α,α-dibromocarbonyl compounds on condensation with phenylacetic acid or thioamide give the furanone or thiazole instead of the expected corresponding 5-bromo products. The mechanistic study have been made to find the reaction path way. 相似文献
34.
Pallavi Singh Rakesh Tripathi Rajiv K. Verma Ganesh C. Nandi Ashutosh Gupta Maya S. Singh 《Phosphorus, sulfur, and silicon and the related elements》2013,188(10):2142-2151
A simple and efficient synthesis of previously unknown benzosubstituted dioxaphosphonines containing a quinoxaline subunit is described. Reasonably good yields of the products, mild reaction conditions, and convenient work-up are the advantages of this method. The procedure does not require any catalyst or activator and can be efficiently achieved via dianion cyclization. All the synthesized compounds have been characterized by satisfactory elemental analyses and spectral (IR, 1H, 13C, 31P NMR, and mass) studies. Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file. 相似文献
35.
Pragati R Sharma Shubham Pandey Vineet K Soni Ganpat Choudhary Rakesh K Sharma 《Supramolecular chemistry》2013,25(9):634-644
ABSTRACTThe current study reveals the synthesis of polymer appended Calix[4]amidocrown-5 with specific binding affinity for iodide at ppm-level. The low detection limits are observed via UV-vis and fluorescence spectroscopy. The time-dependent solution and solid-state 127I NMR studies with 18.8 and 19 ppm shifts, indicate a strong sensing nature of resin towards iodide ion. A significant reduction in surface area and pore volume with higher thermostability of resin after iodide uptake indicated iodide inclusion in the amidocrown cavity. The mechanism of iodide sensing may be governed by noncovalent interactions of NH and OH protons present in amidocrown and phenyl ring as observed in terms of emission enhancement in fluorescence spectroscopy. The binding affinity and stoichiometric determinations are determined by Benesi-Hildebrand and Jobs plots, respectively. 相似文献
36.
Some new biologically potent coumarin derivatives 7a–f, 8a–f, and 9a–f bearing modified pyridine moieties (indeno[1,2-b]pyridine, 4-azaphenanthrene and benzofuro [3,2-b]pyridine) at the sixth position were designed and synthesized. All the synthesized compounds were assayed for their antimicrobial efficiency against Staphylococcus aureus, Bacillus subtilis, Escherichia coli, Salmonella typhi, Candida albicans, and Aspergillus niger. Most of the compounds showed appreciable antimicrobial activity against the tested strains. Compounds 8b, 8c, 9b, 9d, and 9f emerged as most proficient members of the series. The antitubercular activity for all the synthesized compounds was performed against Mycobacterium tuberculosis H37Rv. Compounds 8f, 9b, and 9f exhibited promising antitubercular activity. Consequently, synthesized derivatives were found to be worthy of further investigation. 相似文献
37.
Bhanu Pemmaraju Hitesh K. Agarwal Donghoon Oh Karen W. Buckheit Robert W. Buckheit Jr. Rakesh Tiwari Keykavous Parang 《Tetrahedron letters》2014
A number of 5′-O-dicarboxylic fatty acyl monoester derivatives of 3′-azido-3′-deoxythymidine (zidovudine, AZT), 2′,3′-didehydro-2′,3′-dideoxythymidine (stavudine, d4T), and 3′-fluoro-3′-deoxythymidine (alovudine, FLT) were synthesized to improve the lipophilicity and potentially the cellular delivery of parent polar 2′,3′-dideoxynucleoside (ddN) analogs. The compounds were evaluated for their anti-HIV activity. Three different fatty acids with varying chain length of suberic acid (octanedioic acid), sebacic acid (decanedioic acid), and dodecanedioic acid were used for the conjugation with the nucleosides. The compounds were evaluated for anti-HIV activity and cytotoxicity. All dicarboxylic ester conjugates of nucleosides exhibited significantly higher anti-HIV activity than that of the corresponding parent nucleoside analogs. Among all the tested conjugates, 5′-O-suberate derivative of AZT (EC50 = 0.10 nM) was found to be the most potent compound and showed 80-fold higher anti-HIV activity than AZT without any significant toxicity (TC50 >500 nM). 相似文献
38.
Chelating resins based on biopolymers, specifically cellulose, offers a green analytical method for determination of metal ions at trace levels present in various samples. It offers a fast, accurate and simple method for separation and pre-concentration of metal ions at low concentrations, prior to their determination by instrumental method. Cellulose based chelating resin (CELL-GLY) has been synthesised by immobilising glycine on it. CELL-GLY was used for the determination of trace amounts of Cu2+ and Ni2+ from aqueous solutions before their determination by FAAS. The preparation of CELL-GLY involves simple steps, based on natural and easily available biopolymer cellulose, which makes its use as chelating resin is a green method. The Cu2+ and Ni2+ can be quantitatively recovered from the CELL-GLY in the pH range 4.8–6.9 and 6.9-7.8 respectively with a recovery of more than 95% for each of these metal ions. Recovery of these metal ions using CELL-GLY was quantitative up to 35 °C. The detection limits for copper and nickel by FAAS were 1.20 ppb and 1.40 ppb, respectively. The method was successfully employed for the determination of trace amounts of Cu2+ and Ni2+ in various samples. 相似文献
39.
Sridevi Duggirala Rakesh P. Nankar Selvakumar Rajendran Mukesh Doble 《Applied biochemistry and biotechnology》2014,174(1):283-296
Naturally occurring phytochemicals with reported antibacterial activity were screened for their ability to inhibit the bacterial cell division protein Escherichia coli FtsZ. Among the representative compounds, coumarins inhibit the GTPase and polymerization activities of this protein effectively. Further screening with ten coumarin analogs we identified two promising candidates, scopoletin and daphnetin. The former is found to inhibit the GTPase activity of the protein in a noncompetitive manner. Docking of these coumarins with the modeled protein indicate that they bind to T7 loop, which is different from the GTP-binding site (active site), thereby supporting the experimental data. Lowest binding energy is obtained with scopoletin. 3D QSAR indicates the need for groups such as hydroxyl, diethyl, or dimethyl amino in the 7th carbon for enhanced activity. None of the coumarins exhibited cytotoxicity against NIH/3T3 and human embryonic kidney cell lines. The length of Bacillus subtilis increases in the presence of these compounds probably due to the lack of septum formation. Results of this study indicate the role of coumarins in halting the first step of bacterial cell division process. 相似文献
40.
Archana Chaudhary Nikita Sharma Meena Nagar Shaikh M. Mobin Pradeep Mathur Rakesh Bohra 《Journal of Sol-Gel Science and Technology》2014,70(3):464-472
Modification of [VO(OPri)3] with oximes in different molar ratios, yielded new class of vanadia precursors, [VO{OPri}3?n{L}n] {where, n = 1–3 and LH = C9H16C=NOH (1–3) and (CH3)2C=NOH (4–6)}.All the products are yellow in colour. (1) and (2) are liquid/viscous liquid, while others are solids. Molecular weight measurements of all these derivatives and the ESI-mass spectral studies of (1), (2), (3) and (5) indicate their monomeric nature. 1H and 13C{1H} NMR spectra suggest that the oximato moieties are monodentate in solution which was further confirmed by the 51V NMR signals, appeared in the region expected for tetra-coordinated oxo-vanadium atoms. On ageing, a disproportionation reaction occurs in (1) and some crystals appeared. Single crystal X-ray diffraction analyses of the crystals obtained from (1) as well as from (3) were found to be the same and indicate the presence of side-on {dihapto η 2-(N, O)} binding modes of the oximato ligands, leading to the formation of seven coordination environment around the vanadium atom. Thermogravimetric curve of (1) exhibits multi-step decomposition with the formation of V2O5 as the final product at ~850 °C. Sol–gel transformation of (3) yielded (a) VO2 sintered at 300 °C and (b) V2O5 at 600 °C. Similarly, sol–gel transformations of (1) and (2) yielded V2O5 (c) and (d) at 600 °C, respectively. Formation of monoclinic phase in (a) and orthorhombic phase in (b), (c) and (d) were confirmed by powder XRD patterns. 相似文献