In present study the lead (Pb) levels has been assessed by analyzing the scalp hair and blood samples of mentally retarded/intellectual disabled (MR/ID) children of both genders, age ranged 3–8 years. For comparative purpose, healthy age matched children were also selected. The cloud point extraction of Pb from digested biological samples was carried out by complexed with ammonium pyrrolidinedithiocarbamate. The complexed analyte was subsequently isolated from the aqueous matrix in the micelles of a non-ionic surfactant (Triton X-114). Dilution of the surfactant-rich phase with acidified ethanol was performed after phase separation, and the Pb content was measured by flame atomic absorption spectrometer. Factors affecting the cloud point extraction were evaluated and optimized. The proposed procedure allowed the determination of lead in certified standard and real samples with detection limits of 0.834μgL− and enhancement factor 55. The results were compared with those of healthy children have same age, socioeconomic status and residential areas.