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1.
J Chromatogr Sci ; 60(2): 194-200, 2022 Feb 16.
Artículo en Inglés | MEDLINE | ID: mdl-33948643

RESUMEN

An effectual and stability signifying technique has been validated for the quantitative verification of degradation products in Remdesivir Injectable pharmaceutical products by employing high-performance liquid chromatography with ultraviolet detector. The process was optimized by using an octyldecylsilane chemically bonded column (Kromasil KR100-5 C18; USP L1 phase) with dimensions; 250 mm length × 4.5 mm inner diameter and 5-µm particle size. The method was validated as per International Conference on Harmonization and other current regulatory guidelines for analytical method validation. The anticipated process was found to be robust, accurate, specific, linear, precise, stable and rugged in the concentration ranging from quantification level to 200% of the specification level of specified and unknown degradation impurities. The technique was effectively applied to analyze degradation products in Remdesivir Injectable drug products.


Asunto(s)
Contaminación de Medicamentos , Preparaciones Farmacéuticas , Adenosina Monofosfato/análogos & derivados , Alanina/análogos & derivados , Cromatografía Líquida de Alta Presión/métodos , Estabilidad de Medicamentos , Reproducibilidad de los Resultados
2.
J Chromatogr Sci ; 54(9): 1475-1480, 2016 Oct 17.
Artículo en Inglés | MEDLINE | ID: mdl-27390100

RESUMEN

An efficient and stability-indicating method has been developed and validated for the quantitative determination of tetrahydrofuran (THF), a hydrolytic degradation impurity, in Busulfan injectable pharmaceutical products by using gas chromatograph equipped with a liquid autosampler and a flame ionization detector. The chromatographic separation was performed on a fused silica capillary (Stabilwax; 60 m length × 0.32 mm i.d., 0.5 µm film thickness) column. The methodology was validated in accordance with regulatory guidelines. The proposed method was found to be specific, stable, precise, linear, accurate, robust, and rugged in the concentration range from 4 to 1,080 ppm for THF. The developed method was successfully applied to determine the THF content in Busulfan injectable pharmaceutical products.

3.
J Clin Diagn Res ; 8(10): ZD04-6, 2014 Oct.
Artículo en Inglés | MEDLINE | ID: mdl-25478459

RESUMEN

The management of tooth wear is complex and challenging as it involves multidisciplinary approach. Proper diagnosis and elaborative treatment protocol is necessary to obtain successful and predictable outcome. The objective of full mouth rehabilitation includes identification of the cause, prevention and preservation of the remaining tooth structure. This case report presents the management of the remaining teeth by endodontic and periodontic intervention which was followed by porcelain fused to metal fixed prosthesis, telescopic denture for the upper missing teeth and extra-coronal attachments for the lower missing teeth. Segmental arch technique was utilized for the rehabilitation where anterior teeth were restored first followed by the posterior teeth. Patient had a satisfactory functional and aesthetic results.

4.
Nanotechnology ; 23(9): 095601, 2012 Mar 09.
Artículo en Inglés | MEDLINE | ID: mdl-22322294

RESUMEN

We report selective tunnelling through a nanographene intermolecular tunnel junction achieved via scanning tunnelling microscope tip functionalization with hexa-peri-hexabenzocoronene (HBC) molecules. This leads to an offset in the alignment between the energy levels of the tip and the molecular assembly, resulting in the imaging of a variety of distinct charge density patterns in the HBC assembly, not attainable using a bare metallic tip. Different tunnelling channels can be selected by the application of an electric field in the tunnelling junction, which changes the condition of the HBC on the tip. Density functional theory-based calculations relate the imaged HBC patterns to the calculated molecular orbitals at certain energy levels. These patterns bear a close resemblance to the π-orbital states of the HBC molecule calculated at the relevant energy levels, mainly below the Fermi energy of HBC. This correlation demonstrates the ability of an HBC functionalized tip as regards accessing an energy range that is restricted to the usual operating bias range around the Fermi energy with a normal metallic tip at room temperature. Apart from relating to molecular orbitals, some patterns could also be described in association with the Clar aromatic sextet formula. Our observations may help pave the way towards the possibility of controlling charge transport between organic interfaces.


Asunto(s)
Grafito/química , Modelos Químicos , Modelos Moleculares , Nanoestructuras/química , Semiconductores , Simulación por Computador , Conductividad Eléctrica , Transporte de Electrón , Diseño de Equipo , Análisis de Falla de Equipo , Ensayo de Materiales , Nanoestructuras/ultraestructura , Tamaño de la Partícula
5.
Nanotechnology ; 23(1): 015606, 2012 Jan 13.
Artículo en Inglés | MEDLINE | ID: mdl-22156192

RESUMEN

Molecular self-organization has the potential to serve as an efficient and versatile tool for the spontaneous creation of low-dimensional nanostructures on surfaces. We demonstrate how the subtle balance between intermolecular interactions and molecule-surface interactions can be altered by modifying the environment or through manipulation by means of the tip in a scanning tunnelling microscope (STM) at room temperature. We show how this leads to the distinctive ordering and disordering of a triangular nanographene molecule, the trizigzag-hexa-peri-hexabenzocoronenes-phenyl-6 (trizigzagHBC-Ph6), on two different surfaces: graphite and Au(111). The assembly of submonolayer films on graphite reveals a sixfold packing symmetry under UHV conditions, whereas at the graphite-phenyloctane interface, they reorganize into a fourfold packing symmetry, mediated by the solvent molecules. On Au(111) under UHV conditions in the multilayer films we investigated, although disorder prevails with the molecules being randomly distributed, their packing behaviour can be altered by the scanning motion of the tip. The asymmetric diode-like current-voltage characteristics of the molecules are retained when deposited on both substrates. This paper highlights the importance of the surrounding medium and any external stimulus in influencing the molecular organization process, and offers a unique approach for controlling the assembly of molecules at a desired location on a substrate.

6.
Indian J Pharmacol ; 43(5): 599-600, 2011 Sep.
Artículo en Inglés | MEDLINE | ID: mdl-22022009

RESUMEN

The present study was undertaken to assess the availability of the essential medicines to the people of Kunijarla, Khammam district, AP. This was done in two steps: 1) Comparison of PHC-EML (primary health care essential medicines list) with AP-EML (Andhra Pradesh essential medicines list) and NEML (National essential medicines list); and 2) Assessment of availability of the listed medicines in adequate quantity to meet the needs of people of kunijarla. Results showed that the PHC-EML is on par with AP-EML and NEML. The hospital has 100% availability of the listed medicines; however, there was a need for certain add-on drugs like phenytoin tablets, valproic acid, and activated charcoal since they were prescribed frequently and were not included in PHC-EML. All the drugs which were listed in PHC-EML were being used and none were considered as non-utility supply. Suggestions were given for the revision of PHC-EML according to the criteria for identifying medicines for inclusion in the revised list which was mentioned in NEML.

7.
J Phys Condens Matter ; 22(8): 084025, 2010 Mar 05.
Artículo en Inglés | MEDLINE | ID: mdl-21389401

RESUMEN

The scientific and technical challenges involved in building the planar electrical connection of an atomic scale circuit to N electrodes (N > 2) are discussed. The practical, laboratory scale approach explored today to assemble a multi-access atomic scale precision interconnection machine is presented. Depending on the surface electronic properties of the targeted substrates, two types of machines are considered: on moderate surface band gap materials, scanning tunneling microscopy can be combined with scanning electron microscopy to provide an efficient navigation system, while on wide surface band gap materials, atomic force microscopy can be used in conjunction with optical microscopy. The size of the planar part of the circuit should be minimized on moderate band gap surfaces to avoid current leakage, while this requirement does not apply to wide band gap surfaces. These constraints impose different methods of connection, which are thoroughly discussed, in particular regarding the recent progress in single atom and molecule manipulations on a surface.

8.
Nat Mater ; 8(7): 576-9, 2009 Jul.
Artículo en Inglés | MEDLINE | ID: mdl-19525952

RESUMEN

Gears are microfabricated down to diameters of a few micrometres. Natural macromolecular motors, of tens of nanometres in diameter, also show gear effects. At a smaller scale, the random rotation of a single-molecule rotor encaged in a molecular stator has been observed, demonstrating that a single molecule can be rotated with the tip of a scanning tunnelling microscope (STM). A self-assembled rack-and-pinion molecular machine where the STM tip apex is the rotation axis of the pinion was also tested. Here, we present the mechanics of an intentionally constructed molecule-gear on a Au(111) surface, mounting and centring one hexa-t-butyl-pyrimidopentaphenylbenzene molecule on one atom axis. The combination of molecular design, molecular manipulation and surface atomic structure selection leads to the construction of a fundamental component of a planar single-molecule mechanical machine. The rotation of our molecule-gear is step-by-step and totally under control, demonstrating nine stable stations in both directions.

9.
Phys Rev Lett ; 102(17): 176102, 2009 May 01.
Artículo en Inglés | MEDLINE | ID: mdl-19518800

RESUMEN

Differential conductance (dI/dV) images taken with a low-temperature scanning tunneling microscope enabled the first observation of the electron probability distribution of the molecular orbitals of a pentacene molecule directly adsorbed on a metal surface. The three highest occupied molecular orbitals (HOMO, HOMO-1, and HOMO-2) and the lowest unoccupied molecular orbital are imaged. Thus dI/dV imaging without any intervening insulating layer permits the visualization of a large variety of molecular orbitals in the electronic cloud of a wide-gap molecule physisorbed on a metal surface.

10.
J Phys Chem B ; 112(49): 15718-24, 2008 Dec 11.
Artículo en Inglés | MEDLINE | ID: mdl-19367917

RESUMEN

Femtosecond pump-probe absorption spectroscopy was employed to investigate ultrafast dynamics in various room temperature ionic liquids (RTILs) based on imidazolium cations, i.e., 1,3-dimethylimidazolium iodide ([DMIM]I), 1-butyl-3-methylimidazolium iodide ([BMIM]I), 1-hexyl-3-methylimidazolium iodide ([HMIM]I), 1-hexyl-3-methylimidazolium chloride ([HMIM]Cl), and 1-methyl-3-octylimidazolium chloride ([MOIM]Cl). Immediately after photoexcitation, an induced absorption was observed at various probe wavelengths (555-1556 nm). Afterward, the decay of the induced absorption was found to be independent of the alkyl chain length and viscosity of the ionic liquids. Two alternative mechanisms were proposed to explain the dynamics. In a first scenario excess electrons are generated through one-photon photodetachment of halides analogous to aqueous halide photodetachment. The dynamics in this case were analyzed with the help of a competing kinetic model proposed for geminate recombination in aqueous chloride photodetachment. Alternatively, imidazolium cations may be subject to photoionization. The transient NIR absorption can then be assigned to imidazolium dimer radical cations and/or excess electrons which may be formed upon association of imidazolium radicals with their parent cations. Both scenarios suggest that a thorough explanation of the ultrafast dynamics probably requires the implication of cooperative effects in the ionic liquids upon photoexcitation.

11.
J Phys Condens Matter ; 20(37): 374113, 2008 Sep 17.
Artículo en Inglés | MEDLINE | ID: mdl-21694420

RESUMEN

Ballistic electron emission microscopy (BEEM) experiments on metal-molecule interfaces are briefly reviewed. Results of BEEM experiments with two different orientations of molecules are presented and discussed. Significant differences in uniformity of transport through the molecular layer are found. Implications for device applications are briefly discussed.

12.
J Chem Phys ; 127(18): 184509, 2007 Nov 14.
Artículo en Inglés | MEDLINE | ID: mdl-18020651

RESUMEN

Temperature-dependent investigations of excess electrons in molten solutions of cesium-doped cesium iodide (Cs-CsI) (mole fraction of Cs approximately 0.003) were performed applying femtosecond pump-probe absorption spectroscopy. The pulse-limited induced bleach observed at probe wavelengths from 600 to 1240 nm was attributed to the excitation of equilibrated excess electrons which were initially formed by melting a Cs-CsI mixture. The interpretation of the relaxation process is based on strongly localized polarons that constitute the majority of defect states in this melt. As expected, the bipolaron contribution was insignificant. The time constants (tau1) were found to be temperature dependent confirming our earlier findings in Na-NaI melts that ionic diffusion almost exclusively controls the dynamics of excess electrons in high temperature ionic liquids. Apart from this temperature dependence, the relaxation dynamics of excess electrons do not differ irrespective of the excitation regime (blue or red part of the respective stationary spectra).

13.
Langmuir ; 23(16): 8336-42, 2007 Jul 31.
Artículo en Inglés | MEDLINE | ID: mdl-17602678

RESUMEN

Evaporated pentacene thin films with thicknesses from several nm to 150 nm on gold and silver substrates have been studied by ultraviolet photoelectron spectroscopy (UPS), near-edge X-ray absorption fine structure (NEXAFS), scanning tunneling microscopy (STM), and atomic force microscopy (AFM). It was found that pentacene thin-film structures, particularly their molecular orientations, are strongly influenced by the metal substrates. UPS measurements revealed a distinct change in the valence band structures of pentacene on Au compared to those on Ag, which is attributed to the different packing between adjacent molecules. Using NEXAFS, we observed 74+/-5 degrees and 46+/-5 degrees molecular tilt angles on Ag and Au, respectively, for all measured thicknesses. We propose that pentacene molecules stand up on the surface and form the "thin-film phase" structure on Ag. On Au, pentacene films grow in domains with molecules either lying flat or standing up on the substrate. Such a mixture of two crystalline phases leads to an average tilt angle of 46 degrees for the whole film and the change in valence band structures. STM and distance-voltage (z-V) spectroscopy studies confirm the existence of two crystalline phases on Au with different conducting properties. z-V spectra on the low conducting phase clearly indicate its nature as "thin-film phase".

14.
J Phys Chem B ; 111(18): 4830-6, 2007 May 10.
Artículo en Inglés | MEDLINE | ID: mdl-17269818

RESUMEN

The photochemistry and relaxation dynamics of four room-temperature ionic liquids (RTILs) after ultraviolet (UV) photolysis were investigated by femtosecond pump-probe absorption spectroscopy. A pulse duration-limited rise of the induced absorption in halide-containing RTILs at various probe wavelengths was attributed to the generation of solvated electrons. With continuous irradiation (static conditions), di- and trihalide ion formation became apparent especially below 1000 nm. The formation of trihalide ions was further confirmed by steady-state UV absorption spectroscopy. All RTILs showed a rich photochemistry after UV photolysis leading to the build-up of various long-lived intermediate products as evidenced from the observation that ionic liquids turn yellow upon continuous irradiation. On the other hand, exposing RTILs to the excitation pulse for a short time (rapid-scan method) significantly suppressed the formation of halides. The results suggest that the development of flow-cell systems for highly viscous ionic liquids is urgently needed to quantitatively investigate their ultrafast dynamics.

15.
J Chem Phys ; 125(16): 164512, 2006 Oct 28.
Artículo en Inglés | MEDLINE | ID: mdl-17092110

RESUMEN

Solvated electrons in glycerol were generated via a resonant one-photon photodetachment of the charge-transfer-to-solvent (CTTS) band of I- in glycerol (Gl) after irradiation with a 248 nm excimer laser. Optical absorption spectra of solvated electrons (esolv-) in Gl were recorded as a function of temperature (381

16.
Phys Chem Chem Phys ; 8(27): 3192-6, 2006 Jul 21.
Artículo en Inglés | MEDLINE | ID: mdl-16902711

RESUMEN

The photolytic generation of solvated electrons was observed for the first time in two room temperature ionic liquids (RTILs), trihexyltetradecylphosphonium bis(trifluoromethylsulfonyl)imide (IL) and 1-butyl-1-methyl-pyrrolidinium bis(trifluoromethylsulfonyl)imide (IL). A 70 fs UV-pulse was used to excite the RTILs, while the transient response was monitored in the visible and near-infrared spectral regions. Immediately after excitation, a pulse duration limited rise of the induced absorption indicated the formation of solvated electrons suggesting the existence of pre-formed traps in RTILs. A broad transient absorption spectrum with a full width at half maximum of about 0.9 eV, typical for solvated electrons, was reconstructed from the transient profiles. Wavelength-independent relaxation dynamics at longer delay times suggest a lifetime of solvated electrons in the ns regime in agreement with results from pulse radiolysis studies. Adding 1,1-dimethylpyrrolidinium iodide to IL led to an increase of the UV absorbance and consequently, to an increase of the yield of solvated electrons. Furthermore, this solute is an efficient electron scavenger causing the transients to decay within about 40 ps.


Asunto(s)
Electrones , Iones/química , Rayos Láser , Fotólisis , Absorción , Simulación por Computador , Depuradores de Radicales Libres/química , Imidas/química , Modelos Químicos , Fotoquímica , Piperidinas/química , Pirrolidinas/química , Espectrofotometría Ultravioleta , Temperatura , Rayos Ultravioleta
17.
Indian J Cancer ; 43(2): 86-92, 2006.
Artículo en Inglés | MEDLINE | ID: mdl-16790946

RESUMEN

BACKGROUND: Systemic therapy with radionuclides may be used for the treatment of patients with painful skeletal metastases owing to its efficacy, low cost and low toxicity. Imported radionuclides for pain palliation, like Strontium-89 are expensive; particularly for developing countries. In the Indian scenario, Samarium-153 (Sm-153) is produced in our own reactors and as a result, it is readily available and economical. AIM: We undertook this study to determine the efficacy and toxicity of single-dose Sm-153 ethylenediamine tetramethylene phosphonate as a palliative treatment for painful skeletal metastases. MATERIALS AND METHODS: Eightysix patients with painful skeletal metastases from various primaries, were treated with Sm-153 EDTMP at a dose of 37 MBq/kg. The effects were evaluated according to change in visual analogue pain score, analgesic consumption, Karnofsky performance score, mobility score and blood count tests, conducted regularly for 16 weeks. STATISTICS: Repeated measures analysis. RESULTS: The overall response rates were 73%, while complete response was seen in 12.4%. Reduction in analgesic consumption with improvement in Karnofsky performance score and mobility score, was seen in all responders. Response rates were 80.3 and 80.5% in breast and prostate cancer, respectively. One case, each of Wilms tumor, ovarian cancer, germ cell tumor testis, multiple myeloma, primitive neuroectodermal tumor and oesophageal cancer, did not respond to therapy. No serious side-effects were noted, except for fall in white blood cell, platelet and haemoglobin counts, which gradually returned to normal levels by six-eight weeks. CONCLUSION: Sm-153 EDTMP provided effective palliation in 73% patients with painful bone metastases: the major toxicity was temporary myelosuppression.


Asunto(s)
Analgésicos no Narcóticos/uso terapéutico , Neoplasias Óseas/radioterapia , Compuestos Organometálicos/uso terapéutico , Compuestos Organofosforados/uso terapéutico , Dolor/radioterapia , Cuidados Paliativos , Adolescente , Adulto , Anciano , Anciano de 80 o más Años , Neoplasias Óseas/secundario , China/epidemiología , Femenino , Humanos , Masculino , Persona de Mediana Edad , Neoplasias/patología , Dolor/etiología
18.
J Chem Phys ; 122(20): 204702, 2005 May 22.
Artículo en Inglés | MEDLINE | ID: mdl-15945759

RESUMEN

We have identified a possible electronic origin of metal filaments, invoked to explain the switching behavior of organic devices. Interfaces of two representative organics polyparaphenylene (PPP) and poly(2-methoxy-5-2-ethyl-hexyloxy-1,4-phenylenevinylene) with Ag are investigated using ballistic emission microscopy. Nanometer scale spatial nonuniformity of carrier injection is observed in ballistic electron emission microscopy images of both interfaces. The measured Schottky barrier (SB) appears to be consistent with metal states tailing into the gap of the PPP. We find that the SB values exhibit a distribution, even for the diodes with low ideality factors. The implications of this distribution on the measured physical properties of the diode are discussed, in light of work on devices of similar geometry, published in the literature. We also demonstrate that patches of low SB are likely to nucleate current filaments which can cause local ionization and are reported to be responsible for the switching behavior observed in metal-organic, metal-CuS and Ag-AgSe structures.

19.
Electrophoresis ; 26(6): 1114-21, 2005 Mar.
Artículo en Inglés | MEDLINE | ID: mdl-15706573

RESUMEN

Electroosmotic flow (EOF) was investigated in microfabricated fluidic devices using the current monitoring technique. Current changes ranging from 50 to 130 pA/s were detected. These observations indicate that in microfluidic devices with small reservoir volumes, electrolysis of water influences the fluid transport, giving rise to changes in pH and increase in concentration of ionic species in the fluidic system. As a result of the electrolysis and associated increment in ion concentration, the thickness of the Debye layer and surface potential vary, affecting the overall migration behavior of the solution. The magnitude of EOF and the electrophoretic properties of molecules can no longer be treated as constant/invariant. These temporal anomalies are undesirable during analytical separations and in fluid control applications. A numerical analysis of the impact of the continuous ionic strength increase on the EOF dynamics is presented using well-established conduction and EOF theories. The numerical results are found to be in good agreement with the observed current changes. These results indicate that to improve assay reproducibility, monitoring the electric current is an effective tool to determine whether electrolytic reactions are taking place. Our work also serves to test the numerical accuracy of EOF theories and models.


Asunto(s)
Electrólisis/instrumentación , Microfluídica/instrumentación , Conductividad Eléctrica , Electroforesis Capilar/métodos , Microquímica/instrumentación , Miniaturización , Ósmosis
20.
BMC Ecol ; 5: 1, 2005 Feb 02.
Artículo en Inglés | MEDLINE | ID: mdl-15689236

RESUMEN

BACKGROUND: The Teak defoliator (Hyblaea puera) is a pest moth of teak woodlands in India and other tropical regions (e.g. Thailand) and is of major economic significance. This pest is of major concern as it is involved in complete defoliation of trees during the early part of the growing season. Defoliation does not kill teak trees, but it results in huge amount of timber loss. Teak defoliator outbreaks are a regular annual feature in most teak plantations in India and it is extremely difficult to predict the exact time and place of occurrence of these outbreaks. Evidence from the study of the population dynamics of H. puera indicated habitual, short range movements of emerging moth populations, suggesting that these populations have spread to larger areas, generation after generation, affecting the entire teak plantations. We were therefore interested in investigating the temporal and spatial relationship among various population groups in Nilambur, Kerala (India) and address the cause of outbreak at the landscape level. RESULTS: The populations were classified into 'endemic', 'epicenter' and 'epidemic' populations based on the time of occurrence and size of infestation. We devised a novel method of screening nuclear and mitochondrial DNA polymorphisms using Randomly Amplified Gene Encoding Primers (RAGEP). We have used this method extensively to evaluate the species specificity, reproducibility and to discriminate among the three different characterised populations of teak defoliator. CONCLUSIONS: This method also allowed us to comment with some certainty that the endemic teak defoliator, H. puera do not play a major role in contributing to large-scale infestations. With respect to the hypotheses put forward regarding the origin of outbreaks of the moth, this study confirms the role of migration in outbreak causation, while negating the belief that endemic populations aggregate to cause an epidemic.


Asunto(s)
Productos Agrícolas/parasitología , Lamiaceae/parasitología , Mariposas Nocturnas/genética , Mariposas Nocturnas/fisiología , Animales , Dermatoglifia del ADN , ADN Mitocondrial/genética , Genes de Insecto/genética , Marcadores Genéticos , India , Proteínas Nucleares , Filogenia , Polimorfismo Genético , Dinámica Poblacional , Proteínas Represoras
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