A New Protocol for the Analysis of Pharmaceuticals, Pesticides, and Hormones in Sediments and Suspended Particulate Matter From Rivers and Municipal Wastewaters

We developed a protocol to quantify 12 emerging contaminants (ECs) (pharmaceuticals and hormones) and pesticides extracted from suspended particulate matter (SPM) of river water and municipal wastewaters samples as well as river sediments. The separation of suspended solids was realized using filtration of water samples. We tested a series of six different filter types. The effect of filtration on the concentrations of dissolved contaminants was evaluated to minimize losses of target compounds. The river sediment samples were lyophilized, and both SPM and sediment samples were subjected to ultrasonic extraction combined with C18 cartridge clean-up. Quantifications were realized using mass spectrometry. The method recoveries of all compounds ranged from 38 to 112 % in all studied matrices; poorer recoveries were achieved for sulfamethoxazole and diclofenac (as low as 38 %), whereas the recoveries for all other compounds in the wastewater treatment plant (WWTP) samples were between 68 and 111 %. The detection limits in sediments and SPM from river samples for the 12 analytes varied from 0.7 to 9.4 ng g(-1) and from 21 to 92 ng g(-1) for WWTP SPM samples. All targeted ECs were detected with concentrations ranging from 3 to 5,440 ng g(-1) in the studied matrices with the highest concentrations observed in WWTP SPM samples. A significant portion of the contaminants in a water sample is clearly associated with the suspended particulates. Optimization of water-treatment processes and environmental fate must absolutely consider the fraction of contaminants that is particulate-bound if one hopes to have a reasonable mass balance.