Naled is an organophosphate insecticide that shows relatively low toxicity. While home use has been discontinued, naled is still used in public mosquito eradication programs. Naled can be reduced to dichlorvos, which the EURL included as a target pesticide for the EUPT-CF9. Obelisc R was used to retain naled and separate it from impurities. Obelisc R contains embedded ionic and hydrophobic groups which can assist in fine tuning separations. Method is LC/MS compatible and can be used as a general approach for analyzing naled and other organophosphate insecticides.