Hydrophilic interaction liquid chromatographic tandem mass spectrometric determination of atenolol in human plasma

A hydrophilic interaction liquid chromatographic method with tandem mass spectrometry for the determination of atenolol, a beta-blocking agent, in human plasma has been developed and validated over the curve range of 10--2000 ng/mL. The assay was based on protein precipitation followed by evaporation of the extraction solvent, reconstitution with acetonitrile, and chromatography on an Hypersil silica column (50 x 4.6 mm) using a low aqueous--high organic mobile phase. The mobile phase consists of 85% acetonitrile, 15% water, 0.5% acetic acid and 0.04% trifluoroacetic acid and runs isocratically at a flow rate of 2.0 mL/min. The column ef fluent was split so that 50% of it was transferred into the LC-MS/MS interface operated in positive electrospray ionization mode. The chromatographic run time was 2.0 min per injection. Atenolol and the internal standard, atenolol-d(7), showed a retention time of 1.0 min. The inter-day and intra-day precision and accuracy of the quality control samples were <5.3% relative standard deviation and <8.0% relative error, respectively. To explore the application of the current method for the analysis of other beta-blocking agents, propranolol and metoprolol were tested under the same chromatographic conditions with retention times of 0.68 and 0.75 min, respectively. The present method could be used for therapeutic drug monitoring, pharmacokinetic and drug--drug interaction studies of beta-blocking agents.     

A COMPARISON OF DECAY KINETICS OF PHOTO-PRODUCED ABSORBANCE,EPR, AND LUMINESCENCE CHANGES IN CHROMATOPHORES OF RHODOSPIRRILLUM RUBRUM*

–Quantitative comparison of the decay rate for absorbance photochanges in chromatophores of R. rubrum at the major wavelengths of peaks and troughs (280, 365, 385, 433, 605, 763, 790, 810, 850, 865, 890 nm) reveal no major differences under a variety of sample conditions. In addition, the decay kinetics of EPR phtochange at the two environmental potentials used in this study are identical with the absorbance ph;otochange decay. Decay curves for fresh chromatophores, aged chromatophores, and fresh chromatophores at high ionic strength display a variety of half times and curve shapes. All of these data however, may be fit (within 10 per cent) by the equation x=αe^8.2t+βe^0.18t by merely varying the values of α and β. This is interpreted as meaning that any single trapping site may exist in one of two major forms each of which decays following a first order or pseudo-first order reaction. Although the change in decay pattern upon aging is not reversible, that due to high ionic strength is. The time dependencies for two light emission phenomena have been measured as well as their response to the oxidation state of molecules at the trapping site. A major component of long-lived luminescence follows pseudo-second order kinetics with a half time of 38 msec. A very long lived luminescence shows an increse with time which is nearly proportional to the decay of absorbance photochanges.     

Time resolved resonance fluorescence study of electronically excited iodine atoms, I(5P1/2)

Electronically excited iodine atoms, I(5²P_1/2), have been monitored using time resolved atomic resonance fluorescence. Rate data for quenching by C₃H₈ and CD₄ are presented.     

Metal-ammonia reduction: the ring reduction of aromatic carboxylic esters

Aryl benzoates are reduced to 1,4-dihydroaromatics with Na/NH₃ in the presence of water.     

Management of branch-duct intraductal papillary mucinous neoplasms of the pancreas: observation with MR imaging

Purpose

To evaluate the clinical outcomes of conservative management by observation with MRI of patients with branch-duct intraductal papillary mucinous neoplasms (BD-IPMNs).

Materials and Methods

Twenty-three consecutive patients, who were followed up by MRI with magnetic resonance cholangiopancreatography (MRCP) over a period of more than 9 months after initial MRI examinations, were enrolled in this study. On MRI, number of lesions, the maximum diameter of BD-IPMNs, lesion location, the presence of associated dilatation of main pancreatic duct (MPD), the presence of enhancing mural nodules within the lesion and the presence of interval change were retrospectively reviewed on initial and follow-up MR images in consensus by two radiologists. All patients were evaluated to search for evidence of malignant progression of disease.

Results

The follow-up period ranged from 10 to 96 months (mean, 37 months). On initial MRI with MRCP, a total of 39 lesions were found in 23 patients. The maximum diameter of BD-IPMNs ranged between 6 and 32 mm, with a mean of 12 mm. Thirty-four lesions (87%) of 19 patients remained unchanged in the maximum diameter. Five lesions (13%) of four patients showed an increase in the maximum diameter. Enhancing mural nodules were not found in any individual, neither on the initial MRI study nor on the follow-up studies. There was no patient who had evidence of local aggressive growth of tumor or evidence of metastases to distant sites.

Conclusion

Our study suggests that branch-duct IPMNs without enhancing mural nodules are essentially benign and should be managed nonoperatively through observation by MRI.     

Numerical solution of an inverse initial boundary-value problem for the full time-dependent Maxwell's equations in the presence of imperfections of small volume

We consider the numerical solution, in a three-dimensional bounded domain, of the inverse problem for identifying the location of small electromagnetic imperfections in a medium with homogeneous background. Our numerical algorithm is based on the coupling of a discontinuous Galerkin method for the time-dependent Maxwell's equations, on the exact controllability method and on a Fourier inversion. Several numerical results are given with one and two imperfections and the robustness and accuracy of the numerical method used for the dynamic detection problem are shown.     

Bounded-degree polyhedronization of point sets

In 1994 Grünbaum showed that, given a point set S in ${\mathbb{R}}^3$, it is always possible to construct a polyhedron whose vertices are exactly S. Such a polyhedron is called a polyhedronization of S. Agarwal et al. extended this work in 2008 by showing that there always exists a polyhedronization that can be decomposed into a union of tetrahedra (tetrahedralizable). In the same work they introduced the notion of a serpentine polyhedronization for which the dual of its tetrahedralization is a chain. In this work we present a randomized algorithm running in $O(n{\log }^{6}n)$ expected time which constructs a serpentine polyhedronization that has vertices with degree at most 7, answering an open question by Agarwal et al.     

Conformational Analysis of (S)-4,5,6,7-Tetrahydro-5-Methylimidazo [4,5,1-jk][1,4]-Benzodiazepin-2(1H)-one (R78362)

The solution and solid state conformation of (S)-4,5,6,7-tetrahydro-5-methylimidazo [4,5,1-jk][1,4]-benzodiazepin-2(1H)-one (R78362) have been investigated by low temperature NMR and x-ray diffraction studies. The ¹H NMR spectrum of R78362 shows no evidence of the presence of multiple conformers in the temperature range 340K - 177K. Molecular mechanisms and semiempirical molecular orbital calculations suggest that the nitrogen and ring inversion barriers of R78362 are small and thus a time-averaged ¹H NMR spectrum is probably occurring at 298K. The x-ray diffraction data indicated that there were two independent molecules in the asymmetric unit of the crystal. The two molecules had similar conformations with the benzoimidazole ring being planar and the diazepine ring in a “half-chair” conformation.