A new method is presented for qualitative and quantitative determination of non-metal elements present in organic analyte species immobilized in a sol-gel matrix. Nucleic acids were chosen as well-defined relevant biomolecules for which element ratios could be used for detection and identification. Solid, lyophilized powders of ribose-form nucleotides (AMP, ADP, and ATP) were immobilized/entrapped in a methlytrimethoxysilane (mTMOS) sol-gel matrix and monitored for P (I) 214.9 nm, C (I) 193.0 nm, O (I) 130.2, and N (I) 149.3 nm emission by radio-frequency glow-discharge optical-emission spectroscopy (rf-GD-OES). Using the sol-gel method, analytical blanks were obtained by use of un-doped sol-gels. Empirical formula calculations by use of P (I) and C (I), P (I) and N (I), and P (I) and O (I) emission response ratios demonstrate the versatility of the technique as an element and species-specific detector. Results show there is high correlation between phosphorus and oxygen emission responses and the extent of phosphorylation, demonstrating the capacity of the method to produce vital qualitative and quantitative information for the specific nucleotide. Absolute sub-nanogram detection limits were achieved for all the elements studied.