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A Direct Aqueous Derivatization GSMS Method for Determining Benzoylecgonine Concentrations in Human Urine
Authors:Silvio Chericoni PhD  Fabio Stefanelli PhD  Ylenia Da Valle PhD  Mario Giusiani BSc
Affiliation:1. Section 2. of Forensic Medicine, Department of “Patologia Chirurgica, Medica, Molecolare e dell'Area Critica”, University of Pisa and Azienda Ospedaliero Universitaria Pisana, Pisa, Italy;3. Department of Pharmacy, University of Pisa, Pisa, Italy
Abstract:A sensitive and reliable method for extraction and quantification of benzoylecgonine (BZE) and cocaine (COC) in urine is presented. Propyl‐chloroformate was used as derivatizing agent, and it was directly added to the urine sample: the propyl derivative and COC were then recovered by liquid–liquid extraction procedure. Gas chromatography–mass spectrometry was used to detect the analytes in selected ion monitoring mode. The method proved to be precise for BZE and COC both in term of intraday and interday analysis, with a coefficient of variation (CV) <6%. Limits of detection (LOD) were 2.7 ng/mL for BZE and 1.4 ng/mL for COC. The calibration curve showed a linear relationship for BZE and COC (r2 >0.999 and >0.997, respectively) within the range investigated. The method, applied to thirty authentic samples, showed to be very simple, fast, and reliable, so it can be easily applied in routine analysis for the quantification of BZE and COC in urine samples.
Keywords:forensic science  aqueous derivatization  propyl‐chloroformate  benzoylecgonine  cocaine  human urine  method validation
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