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Quantification of drugs of abuse in municipal wastewater via SPE and direct injection liquid chromatography mass spectrometry



Katrice A. Lippa, Michele M. Schantz, A. Lynn Roberts, Kevin Bisceglia


We present an isotopic-dilution direct injection reversed-phase liquid chromatography-tandem mass spectrometry method for the simultaneous determination of 23 drugs of abuse, drug metabolites, and human-use markers in municipal wastewater. The method places particular emphasis on cocaine; it includes 11 of its metabolites to facilitate assessment of routes of administration and to enhance the accuracy of estimates of cocaine consumption. Four opioids (6-acetylmorphine, morphine, hydrocodone, and oxycodone) are also included, along with five phenylamine drugs (amphetamine, methamphetamine, 3,4-methylenedioxy-methamphetamine, methylbenzodioxolyl-butanamine, and 3,4- methylenedioxy-N-ethylamphetamine) and two human-use markers (cotinine and creatinine). The method is sufficiently sensitive to directly quantify (without preconcentration) 18 analytes in wastewater at concentrations less than 50 ng/L. We also present a modified version of this method that incorporates solid-phase extraction to further enhance sensitivity. The method includes a confirmatory LC separation (selected by evaluating 13 unique chromatographic phases) that has been evaluated using National Institute of Standards and Technology Standard Reference Material 1511 Multi-Drugs of Abuse in Freeze-Dried Urine. Seven analytes (ecgonine methyl ester, ecgonine ethyl ester, anhydroecgonine methyl ester, m-hydroxybenzoylecgonine, p-hydroxybenzoyl-ecgonine, ecgonine, and anhydroecgonine) were detected for the first time in a wastewater sample.
Analytical and Bioanalytical Chemistry


reversed-phase liquid chromatography, mass spectrometry, illicit drugs, wastewater, solid phase extraction, metabolites, isotopic dilution


Lippa, K. , Schantz, M. , , A. and Bisceglia, K. (2010), Quantification of drugs of abuse in municipal wastewater via SPE and direct injection liquid chromatography mass spectrometry, Analytical and Bioanalytical Chemistry, [online], (Accessed June 14, 2024)


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Created September 23, 2010, Updated October 1, 2020