scholarly journals Pushing the analytical limits: new insights into complex mixtures using mass spectra segments of constant ultrahigh resolving power

2019 ◽  
Vol 10 (29) ◽  
pp. 6966-6978 ◽  
Author(s):  
Diana Catalina Palacio Lozano ◽  
Remy Gavard ◽  
Juan P. Arenas-Diaz ◽  
Mary J. Thomas ◽  
David D. Stranz ◽  
...  

A new strategy has been developed for characterization of the most challenging complex mixtures to date, using a combination of custom-designed experiments and a new data pre-processing algorithm.

1978 ◽  
Vol 51 (5) ◽  
pp. 925-939 ◽  
Author(s):  
R. P. Lattimer ◽  
K. R. Welch

Abstract From the results presented here, it is clear that FD-MS is a very effective analytical method for determining molecular weights of polymer chemicals. Molecular ions were the only prominent ions produced in the FD mode of analysis for the series of representative polymer chemicals discussed in this paper. Good molecular ion spectra were obtained even from compounds that are quite unstable, both structurally and thermally. It is also evident, on the other hand, that FD-MS by itself provides only limited chemical structure information. The molecular weight is provided and often nothing else. Fortunately the molecular weight and “chemical intuition” regarding the history of the sample in question are often enough to deduce the structure. If not, then other techniques are available to provide complementary information. Electron impact (EI) mass spectra can be run on the same samples to obtain fragmentation patterns, and other spectro-scopic techniques (infrared and magnetic resonance) can be used to provide detailed structural information. Several application areas can be identified in which FD-MS can play an important role in the characterization of nolymer chemicals in industry. These include chemical identification (molecular weight and structure determination), direct detection of components in mixtures, identification of liquid chromatographic (LC) effluents, characterization of polymer blooms and extracts, identification of vapors from polymer processing, and identification of polymer chemical degradation products. For many of these applications the samples to be analyzed are very complex mixtures of chemical compounds. Electron impact mass spectroscopy is quite limited in its ability to analyze such complex mixtures due to the extensive fragmentation (and perhaps decomposition) that takes place in the ion source. Since molecular ions are normally the only prominent ions formed in the FD mode of analysis, FD-MS can be a very powerful tool for the characterization of polymer chemical mixtures. In summary, field desorption mass spectroscopy can in many cases provide molecular weight and structural data for polymer chemicals heretofore not obtainable by any analytical technique. In addition this information complements well the structural data obtained by magnetic resonance, infrared, and electron impact mass spectroscopy. We therefore feel confident that FD-MS will become increasingly important in the characterization of polymer chemicals in the future.


2020 ◽  
Vol 13 (1) ◽  
pp. 405-430 ◽  
Author(s):  
Diana Catalina Palacio Lozano ◽  
Mary J. Thomas ◽  
Hugh E. Jones ◽  
Mark P. Barrow

The detailed molecular characterization of petroleum-related samples by mass spectrometry, often referred to as petroleomics, continues to present significant analytical challenges. As a result, petroleomics continues to be a driving force for the development of new ultrahigh resolution instrumentation, experimental methods, and data analysis procedures. Recent advances in ionization, resolving power, mass accuracy, and the use of separation methods, have allowed for record levels of compositional detail to be obtained for petroleum-related samples. To address the growing size and complexity of the data generated, vital software tools for data processing, analysis, and visualization continue to be developed. The insights gained impact upon the fields of energy and environmental science and the petrochemical industry, among others. In addition to advancing the understanding of one of nature's most complex mixtures, advances in petroleomics methodologies are being adapted for the study of other sample types, resulting in direct benefits to other fields.


2020 ◽  
Vol 16 (8) ◽  
pp. 1130-1139
Author(s):  
Singaram Sathiyanarayanan ◽  
Chidambaram Subramanian Venkatesan ◽  
Senthamaraikannan Kabilan

Background: Regadenoson is an A2A adenosine receptor agonist that is a coronary vasodilator and commonly used as a pharmacologic cardiac stressing agents. Methods: HPLC method was used for the analysis of related substances. The degraded impurities during the process were isolated and characterized by IR, Mass and NMR spectral analysis. Results: Forced degradation study of regadenoson under conditions of hydrolysis (neutral, acidic and alkaline) and oxidations suggested in the ICH Q1A(R2) was accomplished. The drug showed significant degradation under all the above conditions. On the whole, five novel degradation products were found under diverse conditions along with process related impurities which were not reported earlier. Conclusion: All the degradation products were well characterized by using advanced spectroscopic techniques like IR, 1H NMR, 13C NMR and Mass spectra. The identification of these impurities will be productive for the quality control during the production and stability behavior of the regadenoson drug substance.


1993 ◽  
Vol 48 (12) ◽  
pp. 1781-1783 ◽  
Author(s):  
Abdel-Fattah Shihada

(Me3Sn)3PO3S has been prepared from the reaction of Me3SnCl with Na3PO3S • 12 H2O under cooling in aqueous medium. Its IR and Raman spectra are found to be consistent with a polymeric structure with tetra- and penta-coordinated tin atoms. The 31P NMR and mass spectra of (Me3Sn)3PO3S are reported and discussed.


2021 ◽  
Vol 1 (1) ◽  
Author(s):  
Yongyi Liang ◽  
Qihong Lu ◽  
Zhiwei Liang ◽  
Xiaokun Liu ◽  
Wenwen Fang ◽  
...  

AbstractObligate and non-obligate organohalide-respiring bacteria (OHRB) play central roles in the geochemical cycling and environmental bioremediation of organohalides. Their coexistence and interactions may provide functional redundancy and community stability to assure organohalide respiration efficiency but, at the same time, complicate isolation and characterization of specific OHRB. Here, we employed a growth rate/yield tradeoff strategy to enrich and isolate a rare non-obligate tetrachloroethene (PCE)-respiring Geobacter from a Dehalococcoides-predominant microcosm, providing experimental evidence for the rate/yield tradeoff theory in population selection. Surprisingly, further physiological and genomic characterizations, together with co-culture experiments, revealed three unique interactions (i.e., free competition, conditional competition and syntrophic cooperation) between Geobacter and Dehalococcoides for their respiration of PCE and polychlorinated biphenyls (PCBs), depending on both the feeding electron donors (acetate/H2 vs. propionate) and electron acceptors (PCE vs. PCBs). This study provides the first insight into substrate-dependent interactions between obligate and non-obligate OHRB, as well as a new strategy to isolate fastidious microorganisms, for better understanding of the geochemical cycling and bioremediation of organohalides.


2008 ◽  
Vol 14 (6) ◽  
pp. 571-580 ◽  
Author(s):  
Yang Zhou ◽  
Christopher Booth-Morrison ◽  
David N. Seidman

AbstractThe effects of varying the pulse energy of a picosecond laser used in the pulsed-laser atom-probe (PLAP) tomography of an as-quenched Ni-6.5 Al-9.5 Cr at.% alloy are assessed based on the quality of the mass spectra and the compositional accuracy of the technique. Compared to pulsed-voltage atom-probe tomography, PLAP tomography improves mass resolving power, decreases noise levels, and improves compositional accuracy. Experimental evidence suggests that Ni2+, Al2+, and Cr2+ ions are formed primarily by a thermally activated evaporation process, and not by post-ionization of the ions in the 1+ charge state. An analysis of the detected noise levels reveals that for properly chosen instrument parameters, there is no significant steady-state heating of the Ni-6.5 Al-9.5 Cr at.% tips during PLAP tomography.


2017 ◽  
Vol 62 (1) ◽  
Author(s):  
Priyanka Priyadarshi ◽  
Piyush Dravid ◽  
Inayat Hussain Sheikh ◽  
Sunita Saxena ◽  
Ashish Tandon ◽  
...  

AbstractFilarial parasites are complex mixtures of antigenic proteins and characterization of these antigenic molecules is essential to identify the diagnostically important filaria-specific antigens. In the present study, we have fractionated the somatic extracts from adults of


2003 ◽  
Vol 75 (5) ◽  
pp. 1155-1163 ◽  
Author(s):  
David L. Tabb ◽  
Lori L. Smith ◽  
Linda A. Breci ◽  
Vicki H. Wysocki ◽  
Dayin Lin ◽  
...  

1986 ◽  
Vol 41 (8) ◽  
pp. 971-973 ◽  
Author(s):  
Hartmut Köpf ◽  
Thomas Klapötke

Abstract Bis(/75-cyclopentadienyl)-chloro-selenophenolatotitanium (IV), Bis(?75-cyclopentadienyl)-chloro-selenophenolatozirconium (IV), Bis(//5-cyclopentadienyl)-chloro-selenophenolatohafnium (IV), Bis(^5-cyclopentadienyl)-chloro-selenophenolatotungsten(IV), Mass Spectra The metallocene chloro selenophenolates C p;M Cl(SeChH 5) (Cp = ^5-C5H 5; M = Ti, Z r, Hf, W) were prepared by reaction of Cp2MCl2 with equivalent am ounts of LiSeC6H 5, obtained from phenylselenol and «-butyllithium, and were characterized by 'H NM R, IR and MS data. The fragmentation behaviour of the Ti and W derivatives is elucidated by observing m etastable transi­ tions in the mass spectra.


2005 ◽  
Vol 71 (2) ◽  
pp. 761-765 ◽  
Author(s):  
Corina M. Berón ◽  
Leonardo Curatti ◽  
Graciela L. Salerno

ABSTRACT We designed five degenerate primers for detection of novel cry genes from Bacillus thuringiensis strains. An efficient strategy was developed based on a two-step PCR approach with these primers in five pair combinations. In the first step, only one of the primer pairs is used in the PCR, which allows amplification of DNA fragments encoding protein regions that include consensus domains of representative proteins belonging to different Cry groups. A second PCR is performed by using the first-step amplification products as DNA templates and the set of five primer combinations. Cloning and sequencing of the last-step amplicons allow both the identification of known cry genes encoding Cry proteins covering a wide phylogenetic distance and the detection and characterization of cry-related sequences from novel B. thuringiensis isolates.


Sign in / Sign up

Export Citation Format

Share Document