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Gamez, R.

Publications and source records attributed to Gamez, R..

2 recordsLinked to original sources

LC-MS analysis of RNA through hydrogen bonding of alkylamines

Nucleic acid oligonucleotides represent a promising therapy for treating disease. Production of these biopolymers happens synthetically which can produce impurities concomitant with the desired product. The use of liquid chromatography coupled to high resolution mass spectrometry is a robust analytical technique for determination of sample purity. Traditionally, ion pairing reagents are used to facilitate chromatography separation before sampling with the mass spectrometer. The choice of reagent for analysis can impact the analysis as the length of the oligonucleotide increases. This is in part due to the thermodynamics of transitioning the oligonucleotide from the liquid phase to the gas phase. Here we show that the use of a hydrogen bond donating alkylamine assists with overcoming the energy barrier of phase transition by bonding to the nucleobase as well as the phosphodiester backbone. By increasing the relative hydrophobicity of the oligonucleotide, the transition to the gas phase is increased producing a cleaner mass spectrum. Furthermore, we show that by using a hydrogen bond donating alkylamine, we can remove the fluoroalcohol reagent commonly used in ion pairing mass spectrometry of nucleic acids.

biochemistry↗

Comprehensive Characterization of tRNA by Ultra High-Performance Liquid Chromatography High-Resolution Accurate Mass Spectrometry

Transfer ribonucleic acid (tRNA) are the smallest RNA in the translational triune and contain the greatest density of post-transcriptional modifications than any other RNA types in the cell. Due to the size of tRNA studying these modifications usually entails enzymatic digestion followed by liquid chromatography tandem mass spectrometry (LC-MS/MS). Here we report an advancement in Intact Mass Analysis for identification of tRNA through deconvolution of high resolution accurate mass spectrometry facilitated using a secondary alkylamine as an ion pairing reagent during reverse phase chromatography. We identify in isolated and total S. cerevisiae tRNA 3 CCA variations and show that most tRNA lack a 3 adenosine with the lesser abundant species having the expected CCA termini. We identify a previously unknown stable demethylated Wybutosine intermediate for tRNAPHE and identify low abundant contaminating tRNAs in an isolated tRNAPHE sample. Confirmation of identities was verified through traditional mass spectrometric nucleoside and mass mapping experiments.

biochemistry↗