Confirmation and Quantitation of Cocaine, Benzoylecgonine, Ecgonine Methyl Ester, and Cocaethylene by Gas Chromatography/Mass Spectrometry:Use of Microwave Irradiation for Rapid Preparation of Trimethylsilyl and T-butyldimethylsilyl Derivatives
Open Access
- 1 August 1995
- journal article
- research article
- Published by Oxford University Press (OUP) in American Journal of Clinical Pathology
- Vol. 104 (2) , 187-192
- https://doi.org/10.1093/ajcp/104.2.187
Abstract
The authors developed a technique by which cocaine metabolites as well as cocaethylene can be identified and quantitated using gas chromatography/ mass spectrometry (GC/MS), and deuterated standards of benzoylecgonine, cocaine, ecgonine methyl ester, and cocaethylene as internal standards. The authors used a solid phase extraction (Clean Screen, Worldwide Monitoring Corporation, (Horsham, PA)) technique, and rapid derivatization of metabolites using microwave irradiation before GC/MS analysis. The t-butyldimethylsilyl derivatives (prepared by microwave irradiation in 2.5 minutes, 640 Watts [W]) offered better baseline separation and chromatography than conventional trimethylsilyl derivatives. The assay was linear between 0.87–17.3 μmol/L of benzoylecgonine (250–5,000 ng/mL) concentration, 0.83–16.6 μmol/L of cocaine (250–5,000 ng/mL), 0.79–15.8 μmol/L of cocaethylene (250–5,000 ng/mL) and 1.25–25.1 μmol/L of ecgonine methyl ester (250–5,000 ng/mL). The yields are comparable between the microwave technique and conventional heating.Keywords
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