Pentachlorophenol (PCP) was investigated in freshwater sediments and human breast milk collected from the Pearl River Delta, China. The average level of PCP in river sediments was 7.93 ng/g based on dry weight, ranging from 1.44 to 34.4 ng/g. As to the sediments from fishponds, samples from Zhongshan had the highest PCP levels (37.5 ng/g on average), followed by Dongguan (21.1 ng/g on average) and the least in Shenzhen (3.69 ng/g on average) and Shunde (2.20 ng/g on average). Negative relationship was obtained between the PCP level and pH value in sediment (r=0.553, n=13, p<0.05), while positive relationship was found between the PCP levels and the total organic matter (TOM) levels in sediment (r=0.700, n=17, p<0.01). These results indicated that pH and TOM played important roles during the process of PCP settling down to the sediment. PCP was also detected in human breast milk with an average of 2.15 ng/g. The PCP concentration increased with the age increasing of donors. The estimated PCP body burden for mother, daily and yearly PCP intake of infants ranged from 0.16 to 4.17 mg/person, from 0.26 to 10.23 mug/infant.day and from 0.09 to 3.73 mg/infant.year, respectively.