Polypyrrole/Nylon 6 core-shell Nanofibers mat (PPy/Nylon 6-NFSM), prepared via situ polymerization on nylon6 electrospun nanofibers mat template, was used as an adsorbent to remove Pb2+ from aqueous solutions-To study the adsorption characteristics of PPy/Nylon 6-NFSM on Pb2+, the work focused on two parts, dynamic adsorption and static adsorption-The investigation explored the possibility of PPy/Nylon 6-NFSM as an efficient solid phase extraction (SPE) adsorbent for the separation and enrichment of trace Pb2+ in water samples. The experiment results showed that the maximum static adsorption capacity of PPy/Nylon 6. NFSM for Pb2+ was 542.1 mg/g at 298 K in pH = 10 solution. The adsorption process could be well fitted with the pseudo. second. order kinetic model, the adsorption equilibrium data accorded with Freundlich isotherm model. Under the optimum conditions, PPy/Nylon 6. NFSM was used as adsorbent in SPE coupled with Flame atomic spectrophotometer (AA-7000) for the determination of Pb2+ in water samples. The limits of detection of the method were 1.2 mu g/L (S/N = 3), the recoveries of spiked water samples at concentration of 10 mu g/L were 95.3% - 100.4% with RSD of 1.6%. The method is accurate and sensitive in detection of trace concentrations of Pb2+ in water sample.