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91.
Reversed‐phase liquid chromatography with electrospray mass detection and 1H and 13C NMR characterization of new process‐related impurities,including forced degradants of Efavirenz: Related substances correlated to the synthetic pathway
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In this study, a stability‐indicating reversed‐phase liquid chromatographic electrospray mass spectrometric method was developed and validated for the determination of process‐related impurities and forced degradants of Efavirenz in bulk drugs. Efavirenz was subjected to acid, alkaline hydrolysis, H2O2 oxidation, photolysis, and thermal stress. Significant degradation was observed during alkaline hydrolysis, and the degradants were isolated on a mass‐based purification system and characterized by high‐resolution mass spectrometry, positive electrospray ionization tandem mass spectrometry, and 1H and 13C NMR spectroscopy. Accurate mass measurement and NMR spectroscopy revealed the possible structure of process‐related impurities and degradant under stress conditions. The acceptable separation was accomplished on Waters bondapak C18 column (250 mm × 4.6 mm; 5 μm), using 5 mM ammonium acetate and acetonitrile as a mobile phase in a gradient elution mode at a flow rate of 1.0 mL/min. The eluents were monitored by diode array detector at 247 nm and quantitation limits were obtained in the range of 0.1–2.5 μg/mL for Efavirenz, degradants, and process‐related impurities. The liquid chromatography method was validated with respect to accuracy, precision, linearity, robustness, and limits of detection and quantification as per International Conference on Harmonization guidelines. 相似文献
92.
Chou HL Lai FJ Su WN Pillai KC Sarma LS Hwang BJ 《Langmuir : the ACS journal of surfaces and colloids》2011,27(3):1131-1135
A layer growth mechanism of Pt-Ru bimetallic nanoparticles has been proposed with supporting experiments and calculations by density functional theory (DFT). Elongated Pt atoms on Ru nanoparticles were synthesized via a two-step route, and their structural details were obtained by high-resolution transmission electron microscopy. Because of the intrinsic mismatch of lattice spacing between the two elements, such an unusual growth was analyzed with the DFT simulations to explore the mystery of the growth mechanism. Pt atoms would rearrange the packing order and adjust the Pt-Pt atomic distance, and so do the Ru nanoparticles in order to achieve the optimal energy status of the bimetallic system. The resultant Pt(111) layers could stack on top of the Ru(0001) core more tightly by fitting the pockets left between the Ru atoms. The findings give insight into the formation mechanism of the nanosized Pt-Ru bimetallic catalyst and pave the way for designing bimetallic catalysts with tailored properties at the atomic level. 相似文献
93.
Das MR Sarma RK Saikia R Kale VS Shelke MV Sengupta P 《Colloids and surfaces. B, Biointerfaces》2011,83(1):16-22
A solution-based approach to the synthesis of silver (Ag) nanoparticles by chemical reduction of AgNO(3) in a graphene oxide (GrO) suspension is demonstrated. X-ray diffraction and transmission electron microscopy indicate that the Ag nanoparticles, of size range 5-25nm, were decorated on the GrO sheets. The size and shape of the Ag nanoparticles are dependent on the concentration of the AgNO(3) solution. Antimicrobial activity of such hybrids materials is investigated against the Gram negative bacteria Escherichia coli and Pseudomonous aeruginosa. The bacterial growth kinetics was monitored in nutrient broth supplemented with the Ag nanoparticle-GrO suspension at different conditions. It was observed that P. aeruginosa is comparatively more sensitive to the Ag nanoparticle-GrO suspension. 相似文献
94.
Karan NS Sarkar S Sarma DD Kundu P Ravishankar N Pradhan N 《Journal of the American Chemical Society》2011,133(6):1666-1669
We report a reversible phase transformation of platelet-shaped ZnS nanostructures between wurtzite (WZ) and zinc blende (ZB) phases by reversible insertion/ejection of dopant Mn(II) ions induced by a thermocyclic process. In a reaction flask loaded with WZ ZnS platelets and Mn molecular precursors, during heating Mn ions are incorporated and change the phase of the host nanostructures to ZB; during cooling Mn ions are spontaneously ejected, returning the host nanoplatelets to the original WZ phase. These reversible changes are monitored for several cycles with PL, EPR, XRD, and HRTEM. Interestingly, the (0001) WZ platelets transform to (110) ZB following a nucleation and growth process triggered by a local increase/depletion of the Mn(2+) concentration in the nanocrystals. 相似文献
95.
Koosam Mahendar A. V. S. Sarma P. Raghavaiah Mannepalli Lakshmi Kantam Kenneth J. Klabunde 《Helvetica chimica acta》2011,94(8):1533-1542
Aldol‐type reaction between electron deficient aldehydes and sulfonium salts to afford the corresponding β‐hydroxy α‐sulfanyl esters in moderate‐to‐good yields by using nanocrystalline MgO is described. The sulfanyl group is a useful group for further transformations in organic synthesis. Low Rf‐value isomer is anti‐configured as revealed by X‐ray diffraction study and consistent with the assignment of 1H‐NMR spectrum. 相似文献
96.
An effective and unique method of measuring independently the variations of resistive and capacitive constituents of a practical capacitive transducer using an improved pseudo-active bridge is described. The impedance change in some types of transducers may be due to changes in resistance and/or capacitance either way. Separation of changes in resistance and capacitance results in a better understanding of the transduced variable. The active bridge which separates the changes is suitable for online determination of the two changes. 相似文献
97.
98.
The ruthenium(II) complex [RuI2(Me2SO)4] was synthesized and characterized. The Me2SO ligands are all S-bonded. Reactions of RuI2(Me2SO)4 with ligands containing P, N and S donor atoms have been carried out and the complexes obtained were characterized using different physical methods. [RuI2L4] (L= CH3CN, Me2SO and py), [RuI2(CH3CN)2(PPh3)2] and [RuI2(CS)(PPh3)3] have been synthesized using RuI3 as the source material and characterized as above. 相似文献
99.
Prompt lepton production in hadron collisions is explained in a cluster production model, by assuming that the clusters have a small branching ratio for decay into leptons. The production of low mass and small momentum clusters, normalized to reproduce pionization, can explain the observed large increases of e/π ratio for decreasing pbdT at large angles and the decreasing values of ω/π with increasing xlab near the forward direction. The present model predicts a large increase of the e/ω ratio near the forward direction as xlab increases. 相似文献
100.
In this paper we study an n-unit warm standby system which is needed intermittently with need and no-need periods occurring alternately. The life time of a unit while online and duration of a no-need period are generally distributed random variables while all the others are exponentially distributed. Identifying certain regeneration points, we obtain an expression for the distribution function of the time to the first disappointment. 相似文献