Glyphosate and Glufosinate are phytosanitary products widely used as weed killers, especially in cereal and vegetable crops. This study presents a new analytical approach allowing their quantification and separation on reverse phase thanks to in-vial -addition of a pairing agent. This new strategy provides a method that allows to achieve good retention, separation, and sensibility. A rapid method is set up with 7 min run and easy sample preparation. This sensitivity allows their quantification below 50 µg/kg for fruits and 100 µg/kg whatever the matrix. This method shows good repeatability, yield extraction, and robustness.