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11.
G. Reid Asbury Khalid Al-Saad William F. Siems Richard M. Hannan Herbert H. Hill 《Journal of the American Society for Mass Spectrometry》1999,10(10):983-991
Since the introduction of matrix-assisted laser desorption/ionization (MALDI) mass spectrometry the majority of research has focused on developing analytical methods for the qualitative determination of water soluble biomolecules such as proteins, peptides, carbohydrates, and oligonucleotides. This paper, however, reports the use of MALDI for the analysis of triacylglycerols and develops a new sample preparation method for nonpolar analytes. MALDI enables the rapid analyses of triacylglycerol (TAG) standards and mixtures of whole oils. The new method provides excellent shot to shot reproducibility, making quantification possible. Detection limits were in the mid femtomole range and the resolution was around 2000 which easily separated TAGs differing by one double bond. Sensitivity decreased with increasing molecular weight, causing biased results when analyzing complex mixtures with a significant range of molecular weight. In all cases only sodiated molecules and prompt losses of a fatty acid sodium salt were observed in the spectra. From this information it was possible to identify the three fatty acids on the glycerol backbone. Collision-induced dissociation was carried out on a triacylglycerol which proved to be useful for additional structural information, including the corroboration of the fatty acid components. With MALDI the percent compositions of TAGs in a standard olive oil was accurately determined. Finally, MALDI was used to examine the differences in lipid components between aged and fresh onion seeds, showing the potential of the technique for observing changes in lipid components in seeds. 相似文献
12.
Wenjie Liu Xing Zhang Richard Knochenmuss William F. Siems Herbert H. HillJr. 《Journal of the American Society for Mass Spectrometry》2016,27(5):810-821
A high performance liquid chromatograph (HPLC)was interfaced to an atmospheric drift tube ion mobility time of flight mass spectrometry. The power of multidimensional separation was demonstrated using chili pepper extracts. The ambient pressure drift tube ion mobility provided high resolving powers up to 166 for the HPLC eluent. With implementation of Hadamard transform (HT), the duty cycle for the ion mobility drift tube was increased from less than 1% to 50%, and the ion transmission efficiency was improved by over 200 times compared with pulsed mode, improving signal to noise ratio 10 times. HT ion mobility and TOF mass spectrometry provide an additional dimension of separation for complex samples without increasing the analysis time compared with conventional HPLC. 相似文献
13.
Larry A. Viehland William F. Siems 《Journal of the American Society for Mass Spectrometry》2012,23(11):1841-1854
Moment equations for the motion of trace amounts of charged particles through dilute gases are developed from the Boltzmann equation. A new method for truncating the coupled moment equations is used to develop differential equations governing the moments in successive approximations. The first approximation equations are shown to agree completely with equations known to describe ion motion in drift-tube mass spectrometers, ion mobility spectrometers, ion traps, and collision-dominated ion cyclotron resonance experiments. Applications to differential mobility spectrometers and other devices are also described. 相似文献
14.
Tobias Siems Marc Hellmuth Volkmar Liebscher 《Journal of computational and graphical statistics》2019,28(2):290-298
Within a Bayesian retrospective framework, we present a way of examining the distribution of changepoints through a novel set estimator. For a given level, α, we aim at smallest sets that cover all changepoints with a probability of at least 1 ? α. These so-called smallest simultaneous credible regions, computed for certain values of α, provide parsimonious representations of the possible changepoint locations. In addition, combining them for a range of different α’s enables very informative yet condensed visualizations. Therewith we allow for the evaluation of model choices and the analysis of changepoint data to an unprecedented degree. This approach exhibits superior sensitivity, specificity, and interpretability in comparison with highest density regions, marginal inclusion probabilities, and confidence intervals inferred by stepR. While their direct construction is usually intractable, asymptotically correct solutions can be derived from posterior samples. This leads to a novel NP-complete problem. Through reformulations into an Integer Linear Program we show empirically that a fast greedy heuristic computes virtually exact solutions. Supplementary material for this article is available online. 相似文献
15.
I. Wiedenhöver U. Neuneyer C. Kerskens J. Altmann O. Stuch J. Theuerkauf G. Siems R. Wirowski M. Eschenauer P. von Brentano R. Schubart H. Kluge K. H. Maier 《Zeitschrift für Physik A Hadrons and Nuclei》1993,347(1):71-72
Excited states of the nuclei127Xe and125Xe have been investigated in the inverse kinematic reactions48 Ca(82 Se,(3.5)n) at 275 MeV beam energy with the OSIRIS multidetector system at the VICKSI-accelerator of the HMI Berlin. The level scheme of127Xe was extended up to a level of tentative spin (51/2?). Two excited bands of 3QP-character were observed. For125Xe these structures were extended towards higher spins. Experimental Routhians of selected bands are presented. 相似文献
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A mixture of polydimethylsilicones (Dow Corning 200), average molecular weight 2000 a.m.u., was separated by simultaneous density and temperature-programmed supercritical fluid chromatography and detected by ion mobility detection. Ion mobility spectra were captured by Fourier transform ion mobility spectrometry. Using information from these spectra it was possible to selectively detect a single compound in the complex mixture. A detector temperature investigation demonstrated that, for the efficient transfer of high-molecular-weight compounds from the column to the detector, the interface to the detector must be heated. Using a 50 microns I.D. column, a Guthrie-type restrictor and a detection temperature of 250 degrees C, as many as 70 oligomers were separated and detected. 相似文献