Direct analysis in real time (DART) mass spectrometry is a recently developed innovative technology, which has shown broad applications for fast and convenient analysis of complex samples. Due to the ease of sample preparation, we have recently initiated an investigation of the feasibility of detecting nucleotides and nucleosides using the DART-AccuTOF instrument, which we will refer to as the DART mass spectrometer. Our experimental results reveal that the ions representing the intact molecules of nucleotides are not detectable in either positive-ion or negative-ion mode. Instead, all four natural nucleotides fragment in the DART ion source, and a common fragment ion, [C 5 H 5 O] ϩ (1), is observed, which is probably formed via multiple-elimination reactions. Interestingly, 1 can form adducts with nucleobases in different molar ratios in the DART ion source. In contrast to nucleotides, the ions representing the intact molecules of nucleosides are detected in both positive-ion and negative-ion mode using DART mass spectrometry. Surprisingly, the fragmentation pattern of nucleosides is different from that of nucleotides in the DART ion source. In the cases of nucleosides (under positive-ion conditions), the production of 1 is not observed, indicating that the phosphate group plays an important role for the multiple eliminations observed in the spectra of nucleotides. The in-source reactions described in the present work show the complexity of the conditions in the DART ion source, and we hope that our results illustrate a better understanding about DART mass spectrometry. (J Am Soc Mass Spectrom 2010, 21, 1371-1381
Analysis of substrates directly on solid phase resins without the need for separate cleavage conditions remains an outstanding challenge in the field of solid phase synthesis. We now present the first example of simultaneous cleavage and mass spectrometric analysis of peptides from solid supports using direct analysis in real time (DART) mass spectrometry. We have shown that this method is compatible with a diverse array of solid phase resins, and is suitable for analysis of both peptides and organic substrates.
The real-time Schlieren visualizations introduced in this work provide new insight on the fluid dynamics within the DART-MS sample gap while also helping to identify those experimental parameters requiring optimization for improved transmission.
Based on the concern about the presence of sulfur materials being in drywall (wallboard), a quick and reliable test to confirm the presence or absence of these materials using direct analysis in real time (DART) mass spectrometry in conjunction with an accurate-mass time-of-flight (TOF) mass spectrometer has been developed and is described here. (J Am Soc
In this study, calix[4]arene derivatives (11 -14) bearing a single nucleobase (adenine, thymine, cytosine or guanine) were synthesised via click chemistry. The complexation ability of the synthesised derivatives with alkali metal ions was measured using MALDI-TOF mass spectrometry, and their molecular assembly in CDCl 3 was determined using 1 H NMR. Calix[4]arene derivatives (11 -14) formed 1:1 complexes with all alkali metal ions and the rank order for the complexation selectivity was Rb þ . Cs þ . K þ ø Na þ . Li þ . The attachment of nucleobase at the upper rim of calix[4]arene had little effect on its complexation selectivity for alkali metal ions. Thymine-, adenine-and guanine-calix[4]arenes formed selfassembled structures in CDCl 3 via base-base interactions. In addition, adenine-calix[4]arene (11) bound to thyminecalix[4]arene (12) to form a discrete species via Hoogsteen hydrogen bonding.
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