Determination of estrone and 17α-ethinylestradiol in digested sludge by ultrasonic liquid extraction and high-performance liquid chromatography with fluorescence detection.

Estrone, 17β-estradiol and 17α-ethinylestradiol are increasingly recognised as important micropollutants to be monitored in wastewater treatment plants. These estrogens are retained onto sludge due to their high adsorption and since they are largely used in land applications, the monitoring of these chemicals in sludge samples is of great importance. This study describes a method for the determination of estrone and 17α-ethinylestradiol in fresh sludge samples. After spiking fresh digested sludge with estrone and 17α-ethinylestradiol and maintaining in contact during 5, 30 and 60 min, the freeze-dried samples were subjected to ultrasonic liquid extraction, with methanol and acetone, and analysed by high-performance liquid chromatography with fluorescence detection. The average recoveries obtained for estrone and 17α-ethinylestradiol using the different contact times were 103 ± 3 and 97 ± 4%, respectively. Fresh sludge samples from one waste water treatment plant located in Portugal were analysed and estrone was detected in primary fresh sludge, anaerobic digested sludge and dehydrated sludge at a concentration in the range of 1-4.8 μg/g. The method here developed does not require any sample clean-up, being fast and simple, reliable and inexpensive, making possible its application for monitoring the contamination of sludge with these estrogens.