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Development and validation of an analytical method for the simultaneous determination of cocaine and its main metabolite, benzoylecgonine, in human hair by gas chromatography/mass spectrometry.
Rapid Commun Mass Spectrom. 2008 Oct; 22(20):3320-6.RC

Abstract

A new, simple and rapid procedure has been developed and validated for the determination of cocaine and its main metabolite, benzoylecgonine, in human hair samples. After extraction from within the hair matrix by a mixture of methanol/hydrochloric acid (2:1) at 65 degrees C for 3 h, and sample cleanup by mixed-mode solid-phase extraction (SPE), the extracts were analyzed by gas chromatography/mass spectrometry (GC/MS), after derivatization with N-methyl-N-(trimethylsilyl)trifluoroacetamide with 5% chlorotrimethylsilane. Using a sample size of only 20 mg of hair, limits of detection (LODs) and quantitation (LOQs) were, respectively, 20 and 50 pg/mg for cocaine, and 15 and 50 pg/mg for benzoylecgonine, achieving the cut-off values proposed by the Society of Hair Testing for the analysis of these compounds in hair. The method was found to be linear (weighing factor of 1/x) between the LOQ and 20 ng/mg for both compounds, with correlation coefficients ranging from 0.9974 to 0.9996 for cocaine; and from 0.9981 to 0.9994 for benzoylecgonine. Intra- and interday precision and accuracy were in conformity with the criteria normally accepted in bioanalytical method validation. The sample cleanup step presented a mean absolute recovery greater than 90% for both compounds. The developed method may be useful in forensic toxicology laboratories for the analysis of cocaine and benzoylecgonine in hair samples, taking into account its speed (only 3 h are required for the extraction of the analytes from within the matrix, whereas 5 h or even overnight extractions have been reported) and the low limits achieved (using a single quadrupole mass spectrometer, which is available in most laboratories).

Authors+Show Affiliations

Instituto Nacional de Medicina Legal - Delegação do Sul, Rua Manuel Bento de Sousa, 3, 1150-219 Lisboa, Portugal. mbarroso@blinml.mj.ptNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article

Language

eng

PubMed ID

18819113

Citation

Barroso, M, et al. "Development and Validation of an Analytical Method for the Simultaneous Determination of Cocaine and Its Main Metabolite, Benzoylecgonine, in Human Hair By Gas Chromatography/mass Spectrometry." Rapid Communications in Mass Spectrometry : RCM, vol. 22, no. 20, 2008, pp. 3320-6.
Barroso M, Dias M, Vieira DN, et al. Development and validation of an analytical method for the simultaneous determination of cocaine and its main metabolite, benzoylecgonine, in human hair by gas chromatography/mass spectrometry. Rapid Commun Mass Spectrom. 2008;22(20):3320-6.
Barroso, M., Dias, M., Vieira, D. N., Queiroz, J. A., & López-Rivadulla, M. (2008). Development and validation of an analytical method for the simultaneous determination of cocaine and its main metabolite, benzoylecgonine, in human hair by gas chromatography/mass spectrometry. Rapid Communications in Mass Spectrometry : RCM, 22(20), 3320-6. https://doi.org/10.1002/rcm.3738
Barroso M, et al. Development and Validation of an Analytical Method for the Simultaneous Determination of Cocaine and Its Main Metabolite, Benzoylecgonine, in Human Hair By Gas Chromatography/mass Spectrometry. Rapid Commun Mass Spectrom. 2008;22(20):3320-6. PubMed PMID: 18819113.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Development and validation of an analytical method for the simultaneous determination of cocaine and its main metabolite, benzoylecgonine, in human hair by gas chromatography/mass spectrometry. AU - Barroso,M, AU - Dias,M, AU - Vieira,D N, AU - Queiroz,J A, AU - López-Rivadulla,M, PY - 2008/9/27/pubmed PY - 2008/12/17/medline PY - 2008/9/27/entrez SP - 3320 EP - 6 JF - Rapid communications in mass spectrometry : RCM JO - Rapid Commun Mass Spectrom VL - 22 IS - 20 N2 - A new, simple and rapid procedure has been developed and validated for the determination of cocaine and its main metabolite, benzoylecgonine, in human hair samples. After extraction from within the hair matrix by a mixture of methanol/hydrochloric acid (2:1) at 65 degrees C for 3 h, and sample cleanup by mixed-mode solid-phase extraction (SPE), the extracts were analyzed by gas chromatography/mass spectrometry (GC/MS), after derivatization with N-methyl-N-(trimethylsilyl)trifluoroacetamide with 5% chlorotrimethylsilane. Using a sample size of only 20 mg of hair, limits of detection (LODs) and quantitation (LOQs) were, respectively, 20 and 50 pg/mg for cocaine, and 15 and 50 pg/mg for benzoylecgonine, achieving the cut-off values proposed by the Society of Hair Testing for the analysis of these compounds in hair. The method was found to be linear (weighing factor of 1/x) between the LOQ and 20 ng/mg for both compounds, with correlation coefficients ranging from 0.9974 to 0.9996 for cocaine; and from 0.9981 to 0.9994 for benzoylecgonine. Intra- and interday precision and accuracy were in conformity with the criteria normally accepted in bioanalytical method validation. The sample cleanup step presented a mean absolute recovery greater than 90% for both compounds. The developed method may be useful in forensic toxicology laboratories for the analysis of cocaine and benzoylecgonine in hair samples, taking into account its speed (only 3 h are required for the extraction of the analytes from within the matrix, whereas 5 h or even overnight extractions have been reported) and the low limits achieved (using a single quadrupole mass spectrometer, which is available in most laboratories). SN - 0951-4198 UR - https://www.unboundmedicine.com/medline/citation/18819113/Development_and_validation_of_an_analytical_method_for_the_simultaneous_determination_of_cocaine_and_its_main_metabolite_benzoylecgonine_in_human_hair_by_gas_chromatography/mass_spectrometry_ L2 - https://doi.org/10.1002/rcm.3738 DB - PRIME DP - Unbound Medicine ER -