Solid phase syntheses of peptoid like arylureido compounds and sequencing of isobars without molecular encoding

2019 ◽  
Vol 17 (17) ◽  
pp. 4204-4207
Author(s):  
Kanwal Asif ◽  
Gregory L. O'Brien ◽  
Scott M. Goodman ◽  
Sujit Suwal
Keyword(s):  

Isobaric arylureido peptoids undergo SS1 and SS2 fragmentations in MALDI-TOF MS/MS, thus offering a sequencing mechanism for arylureides without molecular encoding.

2018 ◽  
Vol 2018 ◽  
pp. 1-7 ◽  
Author(s):  
Hoa Thi Le ◽  
Kyu H. Park ◽  
Woong Jung ◽  
Hyung Soon Park ◽  
Tae Woo Kim

We developed a new method for MALDI-TOF MS detection of N-glycans derived from human serum. The synergistic combination of microwave-assisted Girard T derivatization, solid-phase extraction desalting, and an ionic liquid matrix (2, 5-dihydroxybenzoic acid/aniline) (GT-SPE-DHB/An) allowed of more sensitive N-glycans detection than a conventional ionic liquid matrix in MALDI-TOF MS. The superior sensitivity of our method was confirmed by the number of assigned N-glycans in 900–2,000 m/z range. Using our GT-SPE-DHB/An method, we were successfully able to assign 31 glycans. However, with the established method, i.e., DHB/An method, only 15 glycans were assigned. To the best of our knowledge, this GT-SPE-DHB/An method is the first to combine cationic derivatization of N-glycan and ionic liquid matrix for N-glycan analysis in MALDI-TOF MS.


Molecules ◽  
2019 ◽  
Vol 24 (12) ◽  
pp. 2311
Author(s):  
Rosa Terracciano ◽  
Mariaimmacolata Preianò ◽  
Giuseppina Maggisano ◽  
Corrado Pelaia ◽  
Rocco Savino

Improvement in high-throughput MALDI-TOF MS analysis requires practical and efficient sample preparation protocols for high acquisition rates. The use of hexagonal mesoporous silica (HMS) sorbents in combination with MALDI-TOF MS was explored as a versatile tool for peptidomic profiling of clinical specimens difficult to process, but considered important sources of disease biomarkers: synovial fluid and sputum. A rapid and efficient procedure, based on dispersive solid-phase extraction of peptides using commercially available wormhole mesostructured HMS, was tested for: a) pre-concentration of standard peptides in serially diluted solution up to the sub-nanomolar range; b) peptidome profiling of sputum and synovial fluid. The use of HMS, as dispersed sponges, significantly amplified the peptidic repertoire of sputum and synovial fluid by excluding from the adsorptive process large size proteins, which mask and/or suppress peptidome signals. The protocol proposed, as dispersive solid phase extraction, ensures good analytical performances. Moreover, it is economical and rapid, as it avoids the use of less reproducible and prolonged sample preparation procedures, such as the use of ultrafiltration filter devices. These findings may contribute to defining a high-throughput screening MS-based platform for monitoring key peptidic features of difficult to analyse bodily fluids in a clinical setting.


2007 ◽  
Vol 2 ◽  
pp. 117727190700200
Author(s):  
Fabrice Bertile ◽  
Flavie Robert ◽  
Véronique Delval-Dubois ◽  
Sarah Sanglier ◽  
Christine Schaeffer ◽  
...  

Mass spectrometry-based analyses are essential tools in the field of biomarker research. However, detection and characterization of plasma low abundance and/or low molecular weight peptides is challenged by the presence of highly abundant proteins, salts and lipids. Numerous strategies have already been tested to reduce the complexity of plasma samples. The aim of this study was to enrich the low molecular weight fraction of rat plasma. To this end, we developed and compared simple protocols based on membrane filtration, solid phase extraction, and a combination of both. As assessed by UV absorbance, an albumin depletion >99% was obtained. The multistep fractionation strategy (including reverse phase HPLC) allowed detection, in a reproducible manner (CV < 30%-35%), of more than 450 peaks below 3000 Da by MALDI-TOF/MS. A MALDI-TOF/MS-determined LOD as low as 1 fmol/μL was obtained, thus allowing nanoLC-Chip/MS/MS identification of spiked peptides representing ~10–6% of total proteins, by weight. Signal peptide recovery ranged between 5%-100% according to the spiked peptide considered. Tens of peptide sequence tags from endogenous plasma peptides were also obtained and high confidence identifications of low abundance fibrinopeptide A and B are reported here to show the efficiency of the protocol. It is concluded that the fractionation protocol presented would be of particular interest for future differential (high throughput) analyses of the plasma low molecular weight fraction.


2005 ◽  
Vol 77 (6) ◽  
pp. 1580-1587 ◽  
Author(s):  
Nathan G. Hatcher ◽  
Timothy A. Richmond ◽  
Stanislav S. Rubakhin ◽  
Jonathan V. Sweedler

2007 ◽  
Vol 42 (11) ◽  
pp. 1445-1452 ◽  
Author(s):  
Simon Ekström ◽  
Lars Wallman ◽  
Göran Helldin ◽  
Johan Nilsson ◽  
György Marko-Varga ◽  
...  

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