Skip to main content
U.S. flag

An official website of the United States government

Official websites use .gov
A .gov website belongs to an official government organization in the United States.

Secure .gov websites use HTTPS
A lock ( ) or https:// means you’ve safely connected to the .gov website. Share sensitive information only on official, secure websites.

A Streamlined Hydrolysis Procedure for the LC/MS/MS Analysis of Cocaine in Wastewater Samples



Katrice A. Lippa, Kevin Bisceglia, A. Lynn Roberts


We report a streamlined procedure for the routine analysis of cocaine in municipal wastewater. By adding NaOH (to 0.025 M) and incubating wastewater samples at 55 °C for two hours, cocaine and its principal metabolites are quantitatively converted into three products, ecgonine, anhydroecgonine, and norecgonine. Ecgonine, the principal hydrolysis end-product, can be directly determined (without pre-concentration) by liquid chromatography-tandem mass spectrometry (LC/MS/MS) using either reverse phase (RP) or hydrophilic interaction (HILIC) chromatography. In addition to cocaine, three opioids (morphine, hydrocodone, and oxycodone), five phenylamine drugs (amphetamine, methamphetamine, MDMA, MBDB, and MDEA), and two human use markers (cotinine and creatinine) can also be analyzed, as they are stable to hydrolysis. Results obtained by applying the streamlined approach for the analysis of drugs of abuse in untreated municipal wastewater are in excellent agreement with those obtained from the more comprehensive (SPE-)RPLC/MS/MS method described in our companion paper. Seven analytes (ecgonine methyl ester, ecgonine ethyl ester, anhydroecgonine methyl ester, m-hydroxybenzoylecgonine, p-hydroxybenzoylecgonine, ecgonine, and anhydroecgonine) were detected for the first time in an environmental sample.
Environmental Science & Technology


liquid chromatography, mass spectrometry, illicit drugs, wastewater, solid phase extraction, metabolites, hydrolysis, hydrophilic interaction chromatography (HILIC)


Lippa, K. , Bisceglia, K. and , A. (2012), A Streamlined Hydrolysis Procedure for the LC/MS/MS Analysis of Cocaine in Wastewater Samples, Environmental Science & Technology, [online], (Accessed July 18, 2024)


If you have any questions about this publication or are having problems accessing it, please contact

Created January 2, 2012, Updated February 19, 2017