Debris from aquatic macrophytes and algae are important recycling sources of phosphorus (P), which can result in continuing blooms of algae by recycling bioavailable P in the eutrophic lakes. However, knowledge of forms of P in aquatic macrophytes and algae and their contribution to internal loads of P in lakes is limited. Without such knowledge, it is difficult to develop appropriate strategies to remediate and or restore aquatic ecosystems that have become eutrophic. Therefore, in this work, P was extracted from six types of aquatic macrophytes and algae collected from Tai Lake of China and characterized by use of solution 31 P-nuclear magnetic resonance (NMR) spectroscopy. When extracted by 0.5 M NaOH-25 mM EDTA, extraction recovery of total P(TP) and organic P(P o ) exceeded 90 %. Concentrations of P o in algae and aquatic macrophytes were 5552 mg kg −1 and 1005 mg kg −1 and accounted for 56.0 and 47.2 % of TP, respectively. When P o , including condensed P, was characterized by solution 31 P-NMR P o in algae included orthophosphate monoesters (79.8 %), pyrophosphate (18.2 %), and orthophosphate diester (2.0 %), and P o in aquatic macrophytes included orthophosphate monoesters (90.3 %), pyrophosphate (4.2 %), and orthophosphate diester (5.5 %). Additionally, orthophosphate monoesters in algal debris mainly included β-glycerophosphate (44.1 %), α-glycerophosphate (13.5 %), and glucose 6-phosphate (13.5 %). Orthophosphate monoesters in aquatic macrophytes mainly included β-glycerophosphate (27.9 %), α-glycerophosphate (24.6 %), and adenosine 5′ monophosphate (8.2 %). Results derived from this study will be useful in better understanding nutrient cycling, relevant eutrophication processes, and pollution control for freshwater lakes.