Correlation between thermal and mass spectral techniques for the characterization of allenylidene and carbene complexes

2008 ◽  
Vol 71 (1) ◽  
pp. 161-168 ◽  
Author(s):  
Gehad G. Mohamed ◽  
Normen Szesni ◽  
Helmut Fischer
Keyword(s):  
Carbene Complexes ◽  
Spectral Techniques ◽  
Mass Spectral

scholarly journals Mass Spectrometry-Based Characterization of New Spirolides from Alexandrium ostenfeldii (Dinophyceae)

Marine Drugs ◽  
2020 ◽  
Vol 18 (10) ◽  
pp. 505
Author(s):  
Joyce A. Nieva ◽  
Jan Tebben ◽  
Urban Tillmann ◽  
Sylke Wohlrab ◽  
Bernd Krock
Keyword(s):  
Mass Spectrometry ◽  
High Resolution Mass Spectrometry ◽  
Molecular Ions ◽  
Ring System ◽  
The Other ◽  
Spectral Techniques ◽  
Mass Spectral ◽  
Alexandrium Ostenfeldii ◽  
Different Strains

Spirolides belong to a group of marine phycotoxins produced by the marine planktonic dinophyte Alexandrium ostenfeldii. Composed of an imine moiety and a spiroketal ring system within a macrocylcle, spirolides are highly diverse with toxin types that vary among different strains. This study aims to characterize the spirolides from clonal A. ostenfeldii strains collected from The Netherlands, Greenland and Norway by mass spectral techniques. The structural characterization of unknown spirolides as inferred from high-resolution mass spectrometry (HR-MS) and collision induced dissociation (CID) spectra revealed the presence of nine novel spirolides that have the pseudo-molecular ions m/z 670 (1), m/z 666 (2), m/z 696 (3), m/z 678 (4), m/z 694 (5), m/z 708 (6), m/z 720 (7), m/z 722 (8) and m/z 738 (9). Of the nine new spirolides proposed in this study, compound 1 was suggested to have a truncated side chain in lieu of the commonly observed butenolide ring in spirolides. Moreover, there is indication that compound 5 might belong to new spirolide subclasses with a trispiroketal ring configuration having a 6:5:6 trispiroketal ring system. On the other hand, the other compounds were proposed as C- and G-type SPX, respectively. Compound 7 is proposed as the first G-type SPX with a 10-hydroxylation as usually observed in C-type SPX. This mass spectrometry-based study thus demonstrates that structural variability of spirolides is larger than previously known and does not only include the presence or absence of certain functional groups but also involves the triketal ring system.

Synthesis and Characterization of Palladium(II) Complexes with Substituted Dihydrobenzoimidazo Quinazoline Derivatives

2017 ◽  
Vol 13 (2) ◽  
pp. 1-15
Author(s):  
Rita Bhattacharjee Virupaiah Gayathri
Keyword(s):  
Metal Ion ◽  
Synthesis And Characterization ◽  
Planar Geometry ◽  
Conductivity Measurements ◽  
Spectral Techniques ◽  
Mass Spectral ◽  
Square Planar ◽  
Elemental Analyses ◽  
Quinazoline Derivatives

A series of palladium(II) halo complexes of the types [PdX 2 L 2 ].nH 2 O {n = 0, X = Cl, L = L 2 , L 4 and L 5 ; X = Br, L = L 2 ; n = 1, X = Cl, L = L 1 and L 3 } and Pd 2 X 4 L 3 [X = Br, L = L 1 , L 3 , L 4   and L 5 ] were prepared where L is 6-R-5,6- dihydrobenzoimidazo quinazoline (R-Diq; where R = ethyl: L 1 / n or i-propyl: L 2 , L 3 / n or i-butyl: L 4 , L 5 ) and characterized by elemental analyses, conductivity measurements, TGA, infrared, electronic, NMR and mass spectral techniques. Based    on these studies monomeric/dimeric structure with a square planar geometry around the metal ion was proposed for all the complexes. Some of the complexes were investigated for anti-microbial activity.

INFLUENCE OF CLIPPING HEIGHT ON THE NEUTRAL CARBOHYDRATE LEVELS OF ROOT EXUDATES OF ALFALFA PLANTS GROWN UNDER GNOTOBIOTIC CONDITIONS

1972 ◽  
Vol 52 (4) ◽  
pp. 643-649 ◽  
Author(s):  
R. A. HAMLEN ◽  
F. L. LUKEZIC ◽  
J. R. BLOOM
Keyword(s):  
Root Exudates ◽  
Dry Weight ◽  
Root Tissue ◽  
Minor Components ◽  
Flower Buds ◽  
Total Sugars ◽  
Spectral Techniques ◽  
Mass Spectral ◽  
Mature Leaves ◽  
Carbohydrate Levels

Influence of clipping height on neutral carbohydrate levels in root exudates of alfalfa grown gnotobiotically was investigated by gas-chromatographic and mass-spectral techniques. Exudates were obtained from plants that were lightly clipped (removal of flower buds), intermediately clipped (15 cm), and severely clipped (removal of all but four mature leaves). Glucose, inositol, sucrose, and four unidentified (U) components were detected. Fluctuations in the level of sugars were observed in exudates from two sampling periods. Glucose and U1 were most concentrated under light clipping. Levels of inositol and sucrose were maximum under intermediate clipping. Amounts of U3 were greatest from severely clipped plants, whereas levels of U5 remained constant at all cuttings. Concentration of U4 was lowest under severe clipping. U2, present in exudates from seedling plants, was not detected. Quantities of sugars released per gram of dry weight of root tissue were greater under severe clipping. U1 was the major component, with glucose, inositol, and sucrose minor components of the total sugars.

Synthesis and characterization of novel nitroxide organometallic Fischer-type carbene complexes

2013 ◽  
Vol 745-746 ◽  
pp. 57-63 ◽  
Author(s):  
Pascal Le Poul ◽  
Bertrand Caro ◽  
Nolwenn Cabon ◽  
Françoise Robin-Le Guen ◽  
Stéphane Golhen
Keyword(s):  
Synthesis And Characterization ◽  
Carbene Complexes

Syntheses of Alkylated Aromatic Model Compounds To Facilitate Mass Spectral Characterization of Heavy Oils, Resids, and Bitumens

2011 ◽  
Vol 25 (10) ◽  
pp. 4600-4605 ◽  
Author(s):  
M. A. Francisco ◽  
R. Garcia ◽  
B. Chawla ◽  
C. Yung ◽  
K. Qian ◽  
...  
Keyword(s):  
Spectral Characterization ◽  
Heavy Oils ◽  
Model Compounds ◽  
Mass Spectral

scholarly journals Isolation and Structural Characterization of Degradation Products of Aceclofenac by HPLC, HRMS and 2D NMR

2019 ◽  
Vol 31 (4) ◽  
pp. 851-854
Author(s):  
Santhosh Guduru ◽  
V.V.S.R.N. Anji Karun Mutha ◽  
B. Vijayabhaskar ◽  
Muralidharan Kaliyaperumal ◽  
Raghu Babu Korupolu ◽  
...  
Keyword(s):  
Degradation Product ◽  
Degradation Products ◽  
Acid Stress ◽  
2D Nmr ◽  
Stress Conditions ◽  
Preparative Hplc ◽  
Mass Spectral ◽  
2D Nmr Spectra ◽  
The Stability

The stability of aceclofenac under stress conditions was assessed to identify the degradation products. So, it was subjected to stress conditions like acid, base and oxidation, according to ICH guideline Q1A (R2). One degradation product formed when the drug was subjected to acid stress. Three degradation products were formed during the basic stress condition. The drug substance was found to be stable to oxidative stress. The degradants formed during the stress were separated on a C-18 column using gradient preparative HPLC elution. The only product (DP-2) formed during the acid stress and this one is same as of one of the three degradation products (DP-1, DP-2, DP-3) were formed during base stress. 1D and 2D NMR spectra and mass spectral analysis supported the proposed structures for the products. The products DP-2 and DP-3 have been reported earlier but this is the first report of product DP-1 as a degradation product of aceclofenac.

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