Development of a comprehensive LC/MS/MS method for the detection of cocaine and other illicit drugs in municipal wastewater

ENVR 4

Kevin J. Bisceglia, kjb@jhu.edu, Department of Geography and Environmental Engineering and the Analytical Chemistry Division of NIST, Johns Hopkins University and the National Institute of Standards and Technology (NIST), 3400 N. Charles Street, 313 Ames Hall, Baltimore, MD 21218, A. Lynn Roberts, lroberts@jhu.edu, Department of Geography and Environmental Engineering, Johns Hopkins University, 313 Ames Hall, 3400 N. Charles St, Baltimore, MD 21218-2686, and Katrice A. Lippa, katrice.lippa@nist.gov, Analytical Chemistry Division, National Institute of Standards and Technology, 100 Bureau Drive, Mail Stop 8392, Gaithersburg, MD 20899-8392.
We have developed an isotopic dilution SPE-RPLC/MS/MS method for the analysis of 23 illicit drugs, drug metabolites, and human use markers in municipal wastewater. We placed particular emphasis on cocaine, and include eleven of its principal metabolites to maximize our ability to accurately quantify cocaine consumption, and to determine routes of ingestion. This method, which includes a confirmatory LC separation, displays good reproducibility in the analysis of untreated municipal sewage, and is sufficiently sensitive to directly quantify several analytes without pre-concentration. We have also developed a streamlined analysis procedure that collapses cocaine and its metabolites into two hydrolysis products. These products can be directly quantified using NPLC(HILIC)/MS/MS without SPE. This enables shorter chromatographic run times, and reduces uncertainty in sewage-derived estimates of cocaine usage by eliminating the need for assumptions regarding the influence of human metabolism and sewer conditions on metabolite distribution – a principal weakness in current monitoring techniques.