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Quantitation of cocaine, benzoylecgonine, cocaethylene, methylecgonine, and norcocaine in human hair by positive ion chemical ionization (PICI) gas chromatography-tandem mass spectrometry.
J Anal Toxicol. 2000 Oct; 24(7):489-95.JA

Abstract

A total of 30 human head-hair samples were analyzed for cocaine (COC), cocaethylene (CE), benzoylecgonine (BE), methylecgonine (EME), and norcocaine (NCOC) using a sensitive positive ion chemical ionization gas chromatography-tandem mass spectrometry (GC-MS-MS) method. All 30 hair samples had been previously submitted to the laboratory and had confirmed positive for cocaine. Hair samples (20 mg each) were cut into small segments (2-5 mm) and incubated overnight at 45 degrees C in 0.1 N HCl after the addition of 50 microL of an internal standard mix of COC-d3 (1.0 ng/mg), BE-d3 (0.5 ng/mg), EME-d3 (0.25 ng/mg), and NCOC-d3 (0.25 ng/mg). The samples were then extracted with Clean Screen extraction columns from United Chemical Technologies, Inc. The final extract was evaporated to dryness and derivatized with 50 microL of 1,1,1,3,3,3-hexafluoro-2-propanol and 50 microL of trifluoroacetic anhydride at 90 degrees C for 15 min. The derivatized samples were allowed to cool to room temperature, evaporated to dryness, and then reconstituted in 50 microL of ethyl acetate. Parent set masses (unbolded ions) and product ions were m/z 304 and m/z 182 and 82 (COC), m/z 307 and m/z 185 and 85 (COC-d3), m/z 318 and m/z 196 and 82 (CE), m/z 440 and m/z 318 and 105 (BE), m/z 443 and m/z 321 and 105 (BE-d3), m/z 296 and m/z 182, and 82 (EME), m/z 299 and m/z 185 and 85 (EME-d3), m/z 403 and m/z 386 and 105 (NCOC), m/z 406 and m/z 389 and 105 (NCOC-d3). Quantitation was accomplished by calculating the area ratio of the higher mass product ion (underlined ions) of analyte to the respective internal standard based on multilevel calibrations from 0.01 to 10.0 ng/mg. The GC-MS-MS method had a limit of detection of 0.01 ng/mg and a limit of quantitation of 0.05 ng/mg for all five analytes. COC, BE, and EME were detected in all 30 samples, and CE and NCOC were found in 19 and 29 samples, respectively. The average relative percentages of each metabolite normalized to the cocaine concentrations were 12.8%, 15.4%, 1.8%, and 2.5% for BE, CE, EME, and NCOC, respectively.

Authors+Show Affiliations

Associated Pathologists Laboratories, Las Vegas, Nevada 89119, USA.No affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article

Language

eng

PubMed ID

11043651

Citation

Bourland, J A., et al. "Quantitation of Cocaine, Benzoylecgonine, Cocaethylene, Methylecgonine, and Norcocaine in Human Hair By Positive Ion Chemical Ionization (PICI) Gas Chromatography-tandem Mass Spectrometry." Journal of Analytical Toxicology, vol. 24, no. 7, 2000, pp. 489-95.
Bourland JA, Hayes EF, Kelly RC, et al. Quantitation of cocaine, benzoylecgonine, cocaethylene, methylecgonine, and norcocaine in human hair by positive ion chemical ionization (PICI) gas chromatography-tandem mass spectrometry. J Anal Toxicol. 2000;24(7):489-95.
Bourland, J. A., Hayes, E. F., Kelly, R. C., Sweeney, S. A., & Hatab, M. M. (2000). Quantitation of cocaine, benzoylecgonine, cocaethylene, methylecgonine, and norcocaine in human hair by positive ion chemical ionization (PICI) gas chromatography-tandem mass spectrometry. Journal of Analytical Toxicology, 24(7), 489-95.
Bourland JA, et al. Quantitation of Cocaine, Benzoylecgonine, Cocaethylene, Methylecgonine, and Norcocaine in Human Hair By Positive Ion Chemical Ionization (PICI) Gas Chromatography-tandem Mass Spectrometry. J Anal Toxicol. 2000;24(7):489-95. PubMed PMID: 11043651.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Quantitation of cocaine, benzoylecgonine, cocaethylene, methylecgonine, and norcocaine in human hair by positive ion chemical ionization (PICI) gas chromatography-tandem mass spectrometry. AU - Bourland,J A, AU - Hayes,E F, AU - Kelly,R C, AU - Sweeney,S A, AU - Hatab,M M, PY - 2000/10/24/pubmed PY - 2001/3/3/medline PY - 2000/10/24/entrez SP - 489 EP - 95 JF - Journal of analytical toxicology JO - J Anal Toxicol VL - 24 IS - 7 N2 - A total of 30 human head-hair samples were analyzed for cocaine (COC), cocaethylene (CE), benzoylecgonine (BE), methylecgonine (EME), and norcocaine (NCOC) using a sensitive positive ion chemical ionization gas chromatography-tandem mass spectrometry (GC-MS-MS) method. All 30 hair samples had been previously submitted to the laboratory and had confirmed positive for cocaine. Hair samples (20 mg each) were cut into small segments (2-5 mm) and incubated overnight at 45 degrees C in 0.1 N HCl after the addition of 50 microL of an internal standard mix of COC-d3 (1.0 ng/mg), BE-d3 (0.5 ng/mg), EME-d3 (0.25 ng/mg), and NCOC-d3 (0.25 ng/mg). The samples were then extracted with Clean Screen extraction columns from United Chemical Technologies, Inc. The final extract was evaporated to dryness and derivatized with 50 microL of 1,1,1,3,3,3-hexafluoro-2-propanol and 50 microL of trifluoroacetic anhydride at 90 degrees C for 15 min. The derivatized samples were allowed to cool to room temperature, evaporated to dryness, and then reconstituted in 50 microL of ethyl acetate. Parent set masses (unbolded ions) and product ions were m/z 304 and m/z 182 and 82 (COC), m/z 307 and m/z 185 and 85 (COC-d3), m/z 318 and m/z 196 and 82 (CE), m/z 440 and m/z 318 and 105 (BE), m/z 443 and m/z 321 and 105 (BE-d3), m/z 296 and m/z 182, and 82 (EME), m/z 299 and m/z 185 and 85 (EME-d3), m/z 403 and m/z 386 and 105 (NCOC), m/z 406 and m/z 389 and 105 (NCOC-d3). Quantitation was accomplished by calculating the area ratio of the higher mass product ion (underlined ions) of analyte to the respective internal standard based on multilevel calibrations from 0.01 to 10.0 ng/mg. The GC-MS-MS method had a limit of detection of 0.01 ng/mg and a limit of quantitation of 0.05 ng/mg for all five analytes. COC, BE, and EME were detected in all 30 samples, and CE and NCOC were found in 19 and 29 samples, respectively. The average relative percentages of each metabolite normalized to the cocaine concentrations were 12.8%, 15.4%, 1.8%, and 2.5% for BE, CE, EME, and NCOC, respectively. SN - 0146-4760 UR - https://www.unboundmedicine.com/medline/citation/11043651/Quantitation_of_cocaine_benzoylecgonine_cocaethylene_methylecgonine_and_norcocaine_in_human_hair_by_positive_ion_chemical_ionization__PICI__gas_chromatography_tandem_mass_spectrometry_ L2 - https://academic.oup.com/jat/article-lookup/doi/10.1093/jat/24.7.489 DB - PRIME DP - Unbound Medicine ER -