The use of LC-Orbitrap MS for the detection of Fusarium masked mycotoxins: the case of type A trichothecenes

2012 ◽  
Vol 5 (3) ◽  
pp. 271-280 ◽  
Author(s):  
H. Nakagawa ◽  
S. Sakamoto ◽  
Y. Sago ◽  
M. Kushiro ◽  
H. Nagashima

‘Masked mycotoxins’ (mycotoxin glucosides) derived from type A trichothecenes (T-2 toxin and HT-2 toxin) were detected in commercially available maize powder reference material. These novel glucosides were identified as T-2 toxin-glucoside (T2-Glc) and HT-2 toxin-glucoside (HT2-Glc) on the basis of accurate mass measurements of characteristic ions and fragmentation patterns using high-resolution liquid chromatography Orbitrap mass spectrometric analysis. Although their absolute structures were not clarified, 3-OH glucosylation appeared to be the most probable when considering the structure of T-2 toxin and the fragment profiles of each masked mycotoxin. Concomitant detection of deoxynivalenol-3-glucoside (DON-3G) in the same material further supports this probability. According to an extrapolation based on the molar ratio DON-3G/DON (0.059), amounts of T2-Glc and HT2-Glc were estimated to be approximately 24 μg/kg and 41 μg/kg, respectively.

1971 ◽  
Vol 49 (9) ◽  
pp. 1367-1371 ◽  
Author(s):  
J. W. ApSimon ◽  
J. D. Cooney

The mass spectra of seven cyclic N-nitrosamines were examined for characteristic fragmentation patterns. Accurate mass measurements on three of the compounds indicated that the M-17 and M-30 peaks resulted from molecular ion losses of •OH and •NO respectively. The loss of • OH was rationalized in terms of a McLafferty-type rearrangement.


2002 ◽  
Vol 85 (1) ◽  
pp. 50-55 ◽  
Author(s):  
Asit Raksit

Abstract This study describes a fast and accurate method for the sample preparation, identification, and quantitation of nitrilotriacetic (NTA) acid in environmental aqueous samples at a concentration of ppb level. The method is sensitive, specific, and free from the interferences of fatty and amino acids. The tri-n-propyl- and tri-n-butyl-NTA acid esters were prepared by the reaction of n-propyl-HCl and n-butyl-HCl solutions and NTA acid, respectively. The derivatives were analyzed by a gas chromatograph equipped with a mass spectrometric detector. The method detection limit, 0.006 mg/L of each NTA ester, was determined and validated by an analysis of a fortified water sample. The overall recoveries were 103–115%, n = 8. The method was applied to a real sample and a 0.90 mg/L concentration of NTA acid was found. Mass fragmentation patterns of the derivatives are also reported.


2014 ◽  
Vol 2014 ◽  
pp. 1-9 ◽  
Author(s):  
Stanislav D. Anastyuk ◽  
Tatyana I. Imbs ◽  
Pavel S. Dmitrenok ◽  
Tatyana N. Zvyagintseva

The novel highly sulfated (35%) fucoidan fractionCf2, which contained, along with fucose, galactose and traces of xylose and uronic acids was purified from the brown algaCoccophora langsdorfii. Its structural features were predominantly determined (in comparison with fragments of known structure) by a rapid mass spectrometric investigation of the low-molecular-weight fragments, obtained by “mild” (5 mg/mL) and “exhaustive” (maximal concentration) autohydrolysis. Tandem matrix-assisted laser desorption/ionization mass spectra (MALDI-TOF/TOFMS) of fucooligosaccharides with even degree of polymerization (DP), obtained by “mild” autohydrolysis, were the same as that observed for fucoidan fromFucus evanescens, which have a backbone of alternating (1 → 3)- and (1 → 4) linked sulfated at C-2 and sometimes at C-4 of 3-linkedα-L-Fucpresidues. Fragmentation patterns of oligosaccharides with odd DP indicated sulfation at C-2 and at C-4 of (1 → 3) linkedα-L-Fucpresidues on the reducing terminus. Minor sulfation at C-3 was also suggested. The “exhaustive” autohydrolysis allowed us to observe the “mixed” oligosaccharides, built up of fucose/xylose and fucose/galactose. Xylose residues were found to occupy both the reducing and nonreducing termini of FucXyl disaccharides. Nonreducing galactose residues as part of GalFuc disaccharides were found to be linked, possibly, by 2-type of linkage to fucose residues and were found to be sulfated, most likely, at position C-2.


1999 ◽  
Vol 23 (9) ◽  
pp. 584-585
Author(s):  
Aifheli C. Gelebe ◽  
Perry T. Kaye

Fragmentation patterns in the electron-impact (El) mass spectra of benzoxathiepine derivatives are elucidated using a combination of high-resolution and comparative low-resolution mass spectrometric analysis.


2002 ◽  
Vol 2002 (7) ◽  
pp. 321-325 ◽  
Author(s):  
Perry T. Kaye ◽  
Aloysius T. Nchinda ◽  
Christopher A. Gray

Granulosin, a chromone constituent of the bark of Galipea granulosa, and four analogues, all of which exhibit toxicity to the brine shrimp Artemia salina, have been prepared from 2′,3′,4′-trihydroxyacetophenone. High-resolution mass spectrometric analysis has permitted elucidation of the fragmentation patterns exhibited by these systems following electron-impact ionisation.


2019 ◽  
Vol 9 (3) ◽  
pp. 161
Author(s):  
Sung-Eun Cho ◽  
Hyojin Chae ◽  
Hyung-Doo Park ◽  
Sail Chun ◽  
Yong-Wha Lee ◽  
...  

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