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Surface‐activated chemical ionization ion trap mass spectrometry for the analysis of cocaine and benzoylecgonine in hair after extraction and sample dilution
Author(s) -
Cristoni Simone,
Basso Elisa,
Gerthoux Piermario,
Mocarelli Paolo,
Gonella Elisabetta,
Brambilla Maura,
Crotti Sara,
Bernardi Luigi Rossi
Publication year - 2007
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.3107
Subject(s) - benzoylecgonine , chemistry , chromatography , mass spectrometry , gas chromatography–mass spectrometry , chemical ionization , extraction (chemistry) , solid phase extraction , hair analysis , sample preparation , analytical chemistry (journal) , metabolite , ionization , ion , organic chemistry , medicine , biochemistry , alternative medicine , pathology
Surface‐activated chemical ionization (SACI) was employed for the analysis of cocaine and its metabolite, benzoylecgonine, extracted from hair. Following decontamination and acid hydrolysis procedures on the hair sample, the sample solution was diluted (1:10) and directly analyzed by liquid chromatography/surface‐activated chemical ionization multiple collisional stage single reaction monitoring mass spectrometry (LC/SACI‐MS 3 ‐SRM) without solid‐phase extraction (SPE) pre‐purification and concentration procedures. To increase the selectivity of the method, MS 3 was chosen instead of the less selective MS/MS. This data was compared with that achieved using gas chromatography/mass spectrometry (GC/MS), the reference method used by the Italian Government Institute of Health protocol. The limits of detection (LODs) were 0.003 ng/(mg hair) for cocaine and 0.02 ng/(mg hair) for benzoylecgonine and the limits of quantitation (LOQs) were 0.01 ng/(mg hair) for cocaine and 0.04 ng/(mg hair) for benzoylecgonine. The squared correlation coefficient (R 2 ) of the calibration curve was 0.9887–0.9980 for cocaine and 0.9987–0.9997 for benzoylecgonine. The percent accuracy error was 2–5% for both cocaine and benzoylecgonine using the LC/SACI‐MS 3 ‐SRM approach, whereas it was higher for benzoylecgonine (20–25%) using the LC/SACI‐MS/MS‐SRM approach compared with the GC/MS data due to hair matrix contamination. In both cases, high precision was achieved (1–3% precision error), which confirmed the stability of the developed methods. Copyright © 2007 John Wiley & Sons, Ltd.