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Acquisition Mode (acquisition + mode)
Selected AbstractsPhase-rotation in in-vivo localized spectroscopyCONCEPTS IN MAGNETIC RESONANCE, Issue 3 2007Saadallah Ramadan Abstract Phase-rotation is an alternative method to phase-cycling in acquisition of magnetic resonance spectroscopic data. However, there has only been two papers describing its implementation in point resolved spectroscopy (PRESS) and stimulated echo acquisition mode (STEAM) to date. This article aims to introduce and explain the principles of phase-rotation, describe the implementations that were carried out so far in the current literature, compare phase-rotation and phase-cycling experimentally, and introduce the application of phase-rotation in double-quantum filtered (DQF) spectroscopy. © 2007 Wiley Periodicals, Inc. Concepts Magn Reson Part A 30A: 147,153, 2007 [source] Simultaneous determination of simvastatin and simvastatin acid in human plasma by LC-MS/MS without polarity switch: Application to a bioequivalence studyJOURNAL OF SEPARATION SCIENCE, JSS, Issue 2 2008Bhavin N. Patel Abstract A simple, specific and sensitive LC-MS/MS assay for simultaneous determination of simvastatin (SV) and its active ,-hydroxy acid metabolite, simvastatin acid (SVA) in human plasma was developed using a statin analog as internal standard (IS). The method was validated over a dynamic linear range of 0.20,100.00 ng/mL for SV and 0.10,50.00 ng/mL for SVA with correlation coefficient r , 0.9987 and 0.9989, respectively. The analytes and IS were extracted from 500 ,L aliquots of human plasma via liquid-liquid extraction using methyl tert -butyl ether and separated through an Aquasil C18 column (100 mm×2.1 mm, 5 ,m). Detection of analytes and IS was done by MS/MS with a turbo ion spray interface operating in positive ion and selective reaction monitoring acquisition mode. The total chromatographic run time was 3.0 min. Flash freezing of the aqueous phase was an added advantage during liquid-liquid extraction, which considerably reduced time and labour. The method was extensively validated for its accuracy, precision, recovery, stability studies and matrix effect. The method was successfully used for bioequivalence study of 40 mg SV tablet formulation in 12 human subjects under fasting condition. [source] Radial single-shot STEAM MRIMAGNETIC RESONANCE IN MEDICINE, Issue 4 2008Kai Tobias Block Abstract Rapid MR imaging using the stimulated echo acquisition mode (STEAM) technique yields single-shot images without any sensitivity to resonance offset effects. However, the absence of susceptibility-induced signal voids or geometric distortions is at the expense of a somewhat lower signal-to-noise ratio than EPI. As a consequence, the achievable spatial resolution is limited when using conventional Fourier encoding. To overcome the problem, this study combined single-shot STEAM MRI with radial encoding. This approach exploits the efficient undersampling properties of radial trajectories with use of a previously developed iterative image reconstruction method that compensates for the incomplete data by incorporating a priori knowledge. Experimental results for a phantom and human brain in vivo demonstrate that radial single-shot STEAM MRI may exceed the resolution obtainable by a comparable Cartesian acquisition by a factor of four. Magn Reson Med 59:686,691, 2008. © 2008 Wiley-Liss, Inc. [source] MRI of muscular fatMAGNETIC RESONANCE IN MEDICINE, Issue 4 2002Fritz Schick Abstract An MRI technique with high selectivity and sensitivity to the signal components in the chemical shift range of methylene and methyl protons of fatty acids has been developed for noninvasive assessment of muscular fat in vivo. A spoiled gradient-echo sequence with spatial-spectral excitation by six equidistant pulses with 2°-(,9°)-17°-(,17°)-9°-(,2°) and a multi-echo train (TE = 16, 36, 56, 76, 96, and 116 ms) allowed a series of images to be recorded with a receiver bandwidth of 78 Hz per pixel. SIs from phantoms with lipid contents between 0.1% and 100% were compared to those from pure water. Thirty healthy volunteers underwent fat-selective imaging of their lower leg, and parallel localized proton spectroscopy of the tibialis anterior and the soleus muscle by a single-voxel stimulated echo acquisition mode (STEAM) technique (TR = 2 s, TE = 10 ms, TM = 15 ms). Results show a high correlation (r = 0.91) between fat imaging and the spectroscopic approach in the soleus muscle, considering the percentage total fat content of musculature. The correlation coefficient was clearly lower (r = 0.55) in the tibialis anterior muscle due to signal contaminations from adjacent subcutaneous fat in the images, inhomogeneous fat distribution, and generally lower lipid content in this muscle. Applications of the new imaging technique showed marked intra- and interindividual variability in the spatial distribution of lipids in the musculature of the lower leg. No significant correlation of the muscular fat with the thickness of the subcutaneous fat layer was found. In addition, the body mass index does not appear to determine muscular fat content, except in very obese cases. Magn Reson Med 47:720,727, 2002. © 2002 Wiley-Liss, Inc. [source] Rapid differentiation of isobaric and positional isomers of structurally related glycosides from Phytolacca bogotensisRAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 21 2009Guillermo Montoya Through the action of glycosyltransferases, a plant can biosynthetically assemble small different aglycons or 'templates' to various polysaccharides to produce numerous glycoconjugates differing in the type of the attached aglycon, the anomeric configuration of C-1 of the glycosylating sugar, the type of sugar and the different position of attachments of the sugar unit present in the polysaccharide chain. The position of attachments and the anomeric configuration of the different sugar present in the polysaccharide create the opportunity to generate molecules with either the same or very close molecular weights, which have relative structural similarity , forming isobaric and positional isomers. Although isomeric differentiation was once considered outside of the domain of mass spectrometry, this task can now be resolved using tandem mass spectrometry. In a standardized purified glycoconjugate fraction (SPT01) from Phytolacca bogotensis, we report conventional electrospray ionization mass spectrometry and collision-induced dissociation (CID) MS/MS parameters which favored the formation of characteristic product ions. This allowed us to suggest the type of sugar linkages present in a specific glycoconjugate. Ten new glycoconjugate are described from this plant and another twelve known saponins were structurally characterized using the automatic MSn acquisition mode. The differentiation of two pairs of positional isomers and four isobaric glycosides and the production of a library of 30 glycosides present in P. bogotensis were accomplished. Copyright © 2009 John Wiley & Sons, Ltd. [source] A reliable analytical approach based on gas chromatography coupled to triple quadrupole and time-of-flight mass analyzers for the determination and confirmation of polycyclic aromatic hydrocarbons in complex matrices from aquaculture activitiesRAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 13 2009Jaime Nácher-Mestre The potential of gas chromatography coupled to tandem mass spectrometry (GC/MS/MS) with a triple quadrupole analyzer (QqQ) has been investigated for the quantification and reliable identification of sixteen polycyclic aromatic hydrocarbons (PAHs) from the EPA priority list in animal and vegetable samples from aquaculture activities, whose fat content ranged from 5 to 100%. Matrices analyzed included fish fillet, fish feed, fish oil and linseed oil. Combining optimized saponification and solid-phase extraction led to high efficiency in the elimination of interfering compounds, mainly fat, from the extracts. The developed procedure minimized the presence of these interfering compounds in the extracts and provided satisfactory recoveries of PAHs. The excellent sensitivity and selectivity of GC/(QqQ)MS/MS in selected reaction monitoring (SRM) allowed to reach limits of detection at pg/g levels. Two SRM transitions were acquired for each analyte to ensure reliable identification of compounds detected in samples. Confirmation of positive findings was performed by GC coupled to high-resolution time-of-flight mass spectrometry (GC/TOFMS). The accurate mass information provided by GC/TOFMS in full acquisition mode together with its high mass resolution makes it a powerful analytical tool for the unequivocal confirmation of PAHs in the matrices tested. The method developed was applied to the analysis of real-world samples of each matrix studied with the result of detecting and confirming the majority of analytes at the µg/kg level by both QqQ and TOF mass spectrometers. Copyright © 2009 John Wiley & Sons, Ltd. [source] Liquid chromatography/electrospray ionization tandem mass spectrometry validated method for the simultaneous quantification of sibutramine and its primary and secondary amine metabolites in human plasma and its application to a bioequivalence studyRAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 23 2006Deepak S. Jain A high-throughput and sensitive bioanalytical method using liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) has been developed for the estimation of sibutramine and its two metabolites (M1 and M2). The extraction of sibutramine, its metabolites and imipramine (internal standard (IS)) from the plasma involved treatment with phosphoric acid followed by solid-phase extraction (SPE) using a hydrophilic-lipophilic balanced HLB cartridge. The SPE eluate without drying and reconstitution was analyzed by LC/MS/MS, equipped with a with turbo ion spray (TIS) source, operating in the positive and multiple reaction monitoring (MRM) acquisition mode. Sample preparation by this method yielded extremely clean extracts with quantitative and consistent mean recoveries; 95.12% for sibutramine, 92.74% for M1, 95.97% for M2 and 96.60% for the IS. The total chromatographic run time was 3.0,min with retention times of 2.51, 2.13, 2.09,min for sibutramine, M1, M2 and imipramine, respectively. The developed method was validated in human plasma matrix, with a sensitivity of 0.1,ng/mL (coefficient of variance (CV), 2.07%) for sibutramine, 0.1,ng/mL (CV, 3.59%) for M1 and 0.2,ng/mL (CV, 4.93%) for M2. Validation of the method for its accuracy, precision, recovery, matrix effect and stability was carried out especially with regard to real subject sample analysis. The response was linear over the dynamic range 0.1 to 8.0,ng/mL for sibutramine and M1, and 0.2 to 16.0,ng/mL for M2 with correlation coefficients of r,,,0.9959 (sibutramine), 0.9935 (M1) and 0.9943 (M2). The method was successfully applied for bioequivalence studies in 40 human subjects with 15,mg capsule formulations. Copyright © 2006 John Wiley & Sons, Ltd. [source] HPLC-MS of anthraquinoids, flavonoids, and their degradation products in analysis of natural dyes in archeological objectsJOURNAL OF SEPARATION SCIENCE, JSS, Issue 13 2007Izabella Surowiec Abstract LC with MS detection was optimized for sensitive and selective analysis of main classes of natural dyes used in ancient times for dyeing textiles , red anthraquinoids, yellow flavonoids, and known degradation products of flavonols , hydroxybenzoic acids. Fragmentation patterns of both negative and positive molecular ions for the above mentioned compounds were investigated. Three acquisition modes of MS analysis: scanning, SIM, and multiple reaction monitoring (MRM) in both positive and negative ion modes were optimized and compared with each other and with the UV-Vis diode-array detection. Even though in the applied chromatographic system formic acid was used in the mobile phase, SIM in the negative ion mode was the most selective and sensitive detection for all the investigated compounds when both mixtures of standards and analysis of extracts from archeological samples were concerned, with one exception , alizarin, for which MS detection in positive ion mode was more sensitive. Detection limits obtained with MS detection for all investigated compounds except quinizarin were lower than the ones obtained with the diode-array UV-Vis detection, making MS detection the most suitable tool for the analysis of natural dyes and their degradation products in extracts from archeological samples. [source] Optical super-resolution using higher harmonics and different acquisition modes in an aperture tapping SNOMPHYSICA STATUS SOLIDI (B) BASIC SOLID STATE PHYSICS, Issue 8 2010Giovanni Longo Abstract Scanning near field optical microscopy (SNOM) is a well-established technique to obtain a sub-wavelength resolution optical characterization, together with nanometer-scale topography images, on any kind of biological or non-biological sample. Recently we have modified a classical SNOM unit to work in the tapping modality, ensuring stability, versatility and good optical resolution and signal to noise ratio. Exploiting the vertical tip movement, in particular, we were able to access two different optical detection modes: light modulation, which can be obtained by a mechanical chopper or by electronically switching the laser on and off; gap modulation in which the tip's vertical oscillation is used to produce, itself, a modulation of the collected light. Several biological and non-biological samples have been investigated and the data reveal that, despite the signal collected in gap-modulation is at least one order of magnitude smaller than in laser-modulation, resolution, and signal-to-noise ratio in the gap-modulated images is preferable. On the other hand, the higher intensity of the laser-modulation signal allows to deconvolve the optical information at higher harmonics of the tip oscillation frequency. This is a well-known procedure used in the apertureless-SNOM setup to enhance the near-field contribution of the scattered light and reduce the noise content. The interesting results obtained in this Aperture setup are described and commented. [source] Detection of 28 neurotransmitters and related compounds in biological fluids by liquid chromatography/tandem mass spectrometryRAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 9 2006Sophie Bourcier This work presents two liquid chromatography/tandem mass spectrometry (LC/MS/MS) acquisition modes: multiple reaction monitoring (MRM) and neutral loss scan (NL), for the analysis of 28 compounds in a mixture. This mixture includes 21 compounds related to the metabolism of three amino acids: tyrosine, tryptophan and glutamic acid, two pterins and five deuterated compounds used as internal standards. The identification of compounds is achieved using the retention times (RT) and the characteristic fragmentations of ionized compounds. The acquisition modes used for the detection of characteristic ions turned out to be complementary: the identification of expected compounds only is feasible by MRM while expected and unexpected compounds are detected by NL. In the first part of this work, the fragmentations characterizing each molecule of interest are described. These fragmentations are used in the second part for the detection by MRM and NL of selected compounds in mixture with and without biological fluids. Any preliminary extraction precedes the analysis of compounds in biological fluids. Copyright © 2006 John Wiley & Sons, Ltd. [source] | |||||||||||||