A Rapid and Sensitive LC–MS Method for Determination of Ezetimibe Concentration in Human Plasma: Application to a Bioequivalence Study

A selective and highly sensitive high performance liquid chromatography-electrospray ionization mass spectrometry method has been developed for determination of ezetimibe concentrations in human plasma. Ezetimibe was extracted from plasma with ethyl acetate followed by evaporation of the organic layer and, then, reconstitution of the residue in mobile phase before injection to chromatograph. The mobile phase consisted of acetonitrile-ammonium acetate (10 mM, pH 3.0), 75:25 (v/v). An aliquot of 10 μL was chromatographically analyzed on a prepacked Zorbax XDB-ODS C₁₈ column (2.1 × 100 mm, 3.5 micron). Detection of analytes was achieved by mass spectrometry with atmospheric pressure chemical ionization (APCI) interface in the negative ion mode operated under the multiple-reaction monitoring mode (m/z transition: ezetimibe 408–271). Standard curves were linear (r = 0.998) over the wide ezetimibe concentration range of 0.05–30.0 ng mL^?1 with acceptable accuracy and precision. The limit of detection was 0.02 ng mL^?1. The validated LC–APCI–MS method has been used successfully throughout a bioequivalence study on an ezetimibe generic product in 24 healthy male volunteers.     

Background correction by wavelength modulation using a microcomputer in atomic emission spectrometry

An Apple IIe microcomputer was employed to correct the background radiation in electrothermal atomization atomic emission spectrometry (ETA-AES). In ETA-AES, black-body radiation from the atomizer as well as any broadband molecular emission should be corrected to obtain an atomic signal alone. A quartz plate run by a G325D galvanometric motor was placed before the exit slit of a 256 mm Littrow monochromator. Improvements by a novel pulsed 3-step square waveform are demonstrated compared with the ordinatry 3-step square waveform. A soft delay was also applied in order to avoid taking data at transition stages of the quartz plate. A line and a continuum source are used to simulate offsetting of the DC component of the signal prior to the ADC. This provides a better utilization of the full dynamic range of the converter.     

Tandem dispersive liquid–liquid microextraction coupled with micro-sampling flame atomic absorption spectrometry for rapid determination of lead(II) and cadmium(II) ions in environmental water samples

ABSTRACT

Tandem dispersive liquid liquid microextraction coupled with micro - sampling flame atomic absorption spectrometry for rapid determination of lead2 and cadmium2 ions in environmental water samples. A simple method termed as tandem dispersive liquid–liquid microextraction coupled with micro-sampling flame atomic absorption spectrometry is used for determination of the lead(II) and cadmium(II) ions in different environmental water samples. According to the proposed method, the target analytes are extracted from an aqueous sample solution (10 mL) into a micro-volume of an organic solvent, and then they are selectively back-extracted into an aqueous acceptor solution (150 μL) to increase the compatibility of the extractant phase with a final analyser system and provide a suitable enrichment factor. The developed method is very fast, implemented in just about 7 min, and provides a high sample clean-up. The factors influencing the extraction efficiency including the type and volume of the organic solvent, pH and volume of the acceptor solution, and number of extractions are thoroughly examined and optimised. Under the optimal experimental conditions, the developed method provides a good linearity (in the range of 0.4–300 ng mL^?1 (R² ≥ 0.994)), and low limits of detection (in the range of 0.07–0.31 ng mL^?1). Finally, the method is successfully applied for the direct determination of the understudied analytes in the river, dam, and well water samples.     

On the thermodynamics of some generalized second-grade fluids

The generalized second-grade fluids, which have been used for modeling the creep of ice and the flow of coal-water and coal-oil slurries, are among the simplest non-Newtonian fluid models that can describe shear-thinning/thickening and exhibit normal stress effects. In this article, we conduct thermodynamic analysis on a class of generalized second-grade fluids, one distinguishing feature of which is the existence of a constitutive function Φ that describes frictional heating. We work within the framework of Serrin’s original formulation of neoclassical thermodynamics, where internal energy and entropy functions, if they exist for a continuous body at all, are to be derived from the classical First Law and (quantitatively reformulated) Second Law of thermodynamics for cycles. For the class of generalized second-grade fluids in question, we show from the First Law that an internal energy density u exists, and we derive the equation of energy balance; from the Second Law, we demonstrate the existence of an entropy density s and derive the Clausius–Duhem inequality that it satisfies. We obtain explicit expressions for u, s and the frictional heating Φ, and derive thermodynamic restrictions on the material functions of temperature μ, α ₁, and α ₂ that appear in the constitutive relation for the Cauchy stress. For the special case of second-grade fluids, our expressions for u and s agree with those which Dunn and Fosdick [6] derived under the theoretical framework of the rational thermodynamics of Coleman and Noll.     

Three new phosphoric triamides with a [C(O)NH]P(O)[N(C)(C)]2 skeleton: a database analysis of C—N—C and P—N—C bond angles

In N,N,N′,N′‐tetraethyl‐N′′‐(4‐fluorobenzoyl)phosphoric triamide, C₁₅H₂₅FN₃O₂P, (I), and N‐(2,6‐difluorobenzoyl)‐N′,N′′‐bis(4‐methylpiperidin‐1‐yl)phosphoric triamide, C₁₉H₂₈F₂N₃O₂P, (II), the C—N—C angle at each tertiary N atom is significantly smaller than the two P—N—C angles. For the other new structure, N,N′‐dicyclohexyl‐N′′‐(2‐fluorobenzoyl)‐N,N′‐dimethylphosphoric triamide, C₂₁H₃₃FN₃O₂P, (III), one C—N—C angle [117.08 (12)°] has a greater value than the related P—N—C angle [115.59 (9)°] at the same N atom. Furthermore, for most of the analogous structures with a [C(=O)NH]P(=O)[N(C)(C)]₂ skeleton deposited in the Cambridge Structural Database [CSD; Allen (2002). Acta Cryst. B 58 , 380–388], the C—N—C angle is significantly smaller than the two P—N—C angles; exceptions were found for four structures with the N‐methylcyclohexylamide substituent, similar to (III), one structure with the seven‐membered cyclic amide azepan‐1‐yl substituent and one structure with an N‐methylbenzylamide substituent. The asymmetric units of (I), (II) and (III) contain one molecule, and in the crystal structures, adjacent molecules are linked via pairs of N—H...O=P hydrogen bonds to form dimers.     

Simple and sensitive high-performance liquid chromatography method for the quantitation of indinavir in rat plasma and central nervous system

A simple and sensitive RP-HPLC method using UV detection (215 nm) was developed for the determination of indinavir concentrations in rat plasma, cerebrospinal fluid (CSF), and brain tissue homogenates. Biological samples were processed using a combination of acid pretreatment and liquid-liquid extraction with verapamil used as the internal standard. This method produced a linear response throughout the indinavir concentration range of 0.05-30 microM in plasma and 0.05-2.5 microM in CSF and brain with a LOD of 12.5 nM for plasma and CSF, and 6.25 nM for brain homogenate. Due to its high sensitivity, this assay is particularly useful for the quantitative determination of indinavir concentrations in brain and CSF.     

NEURAL NETWORK ANALYSIS APPLICATION TO PERMEABILITY DETERMINATION OF FIBERGLASS AND CARBON PREFORMS

Preform permeability is an important process parameter in liquid injection molding of composite parts.This parameter is currently determined with time consuming and expensive experimental procedures.This paper presents the application of a back-propagation neural network to predicting fiber bed permeability of three types of reinforcement mats. Resin flow experiments were performed to simulate the injection cycle of a resin transfer molding process.The results of these experiments were used to prepare a ...     

Cavity enhancement of the magneto-optic Kerr effect in glass/Al/SnO2/PtMnSb/SnO2 structure

The cavity enhancement effect of the transparent semiconductor SnO₂ on the magneto-optical Kerr response of the glass/Al/SnO₂/PtMnSb/SnO₂ multilayer structure has been investigated using a matrix method. It has been demonstrated that device optimization leads to large Kerr rotation and figure of merit (FOM) with a vanishing ellipticity in the visible portion of the electromagnetic spectrum, especially at short wavelengths. This optimization is of interest in view of optical data storage technology. Using numerical simulations, we have also shown that in the optimum condition, the device readout parameters behave smoothly against the design variables.     

Heat transfer and Couette flow of a chemically reacting non‐linear fluid

In this paper we study the flow and heat transfer in a chemically reacting non‐linear fluid between two long horizontal parallel flat plates that are at different temperatures. The top plate is sheared, whereas the bottom plate is fixed. The fluid is modeled as a generalized power‐law fluid whose viscosity is also assumed to be a function of the concentration. The effects of radiation are neglected. The equations are made dimensionless and the boundary value problem is solved numerically; the velocity and temperature profiles are obtained for various dimensionless numbers. Published in 2009 by John Wiley & Sons, Ltd.     

Electroless deposition of silver nanofractals on copper wire by galvanic displacement as a simple technique for preparation of porous solid‐phase microextraction fibers

A novel and porous solid‐phase microextraction fiber was prepared by quick and simple galvanic displacement reaction and applied to the determination of some polycyclic aromatic hydrocarbons in sunflower oil. The parameters affecting the porosity and thickness of the fiber, and parameters affecting the extraction efficiency, including the extraction time, temperature, and ionic strength, were investigated and optimized. The morphology of prepared fiber was characterized by optical and scanning electron microscopy and thermal and chemical stabilities of the fiber were studied. Under the optimum conditions, the limits of detection ranged between 0.1 ng/mL for pyrene to 1.2 ng/mL for anthracene, and LOQ ranged between 0.3 ng/mL for pyrene to 3.6 ng/mL for anthracene. The relative standard deviations, including repeatability (within fibers) and reproducibility (between fibers), varied between 3.2–8.9 and 5.6–9.8%, respectively.