Development of a hydrophilic interaction-based procedure for the extraction, separation, and determination of therapeutic oligonucleotides

Data have been deposited on the development of dSPE HILIC MS/MS procedure for therapeutic, modified oligonucleotides. A comprehensive retention study examining the effects of mobile phase composition (type of salt, its concentration and pH) and temperature on retention and peak shape was conducted for zwitterionic and amide column. The optimization of mass spectrometry parameters was performed to obtain the high sensitivity. Repository contains data for design of experiments approach. Validated procedure was applied for the analysis of oligonucleotides in enriched serum extracts. Newly synthesized amide-based sorbent was used for dSPE. conditions for adsorption and desorption, which are driven by weak ion-exchange mechanism and thus by pH change, were optimized to obtain the highest recoveries. The repository contains data for the optimization of extraction procedure and its application to serum.