Abstract
The analytical system used for determination of 22 illicit and licit drugs by gas chromatography–mass spectrometry following liquid–liquid extraction has been extended with an additional extraction step with n-butyl acetate:CH2Cl2 = 1:8 to determine benzoylecgonine from the same oral fluid, blood, or urine samples. The extraction recovery of benzoylecgonine was 39.7% for oral fluid, 14.9% for blood, and 26.7% for urine; the cutoffs were 25, 8.0, and 8.0 ng/ml, respectively. The method was fully validated and proved suitable in further proficiency tests and for analysis of 2738 oral fluid, 197 blood, and 1298 urine samples.
Similar content being viewed by others
References
Kankaanpaa A, Gunnar T, Ariniemi K, Lillsunde P, Mykkanen S, Seppala T (2004) Single step procedure for gas chromatography-mass spectrometry screening and quantitative determination of amphetamine-type stimulants and related drugs in blood, serum, oral fluid and urine samples. J Chromatogr B 810:57–68. doi:10.1016/jchromb.2004.07.035
Gunnar T, Ariniemi K, Lillsunde P (2005) Determination of 14 benzodiazepines and hydroxyl metabolites, zaleplon and zolpidem as tert-butyldimethylsilyl derivatives compared with other common silylating reagents in whole blood by gas chromatography–mass spectrometry. J Chromatogr B 818:175–189. doi:10.1016/jchromb.2004.12.032
Gunnar T, Ariniemi K, Lillsunde P (2005) Validated toxicological determination of 30 drugs of abuse as optimized derivatives in oral fluid by long column fast gas chromatography/electron impact mass spectrometry. J Mass Spectrom 40:739–753. doi:10.1002/jms.846
Kolbrich EA, Barnes AJ, Gorelick DA, Boyd SJ, Cone EJ, Huestis MA (2006) Major and minor metabolites of cocaine in human plasma following controlled subcutaneous cocaine administration. J Anal Toxicol 30:501–510
Kato K, Hillsgrove M, Weinhold L, Gorelik DA, Darwin WD (1993) Cocaine and metabolite excretion in saliva under stimulated and nonstimulated conditions. J Anal Toxicol 17:338–341
Gerlits J (1993) GC/MS quantitation of benzoylecgonine following liquid–liquid extraction of urine. J Forensic Sci 38:1210–1214
Álvarez I, Palos F, Bermejo AM, Fernández P, Tabernero MJ (2006) Simultaneous determination of methadone, cocaine and their metabolites in urine by GC–MS. Anal Lett 39:1393–1399. doi:10.1080/00032710600668699
Thompson LK, Yousefnejad D, Kumor K, Sherer M, Cone EJ (1987) Confirmation of cocaine in human saliva after intravenous use. J Anal Toxicol 11:36–38
Cámpora P, Bermejo AM, Tabernero MJ, Fernández P (2003) Quantitation of cocaine and its major metabolites in human saliva using gas chromatography–positive chemical ionization–mass spectrometry (GC–PCI–MS). J Anal Toxicol 27:270–274
Clauwaert K, Decaestecker T, Mortier K, Lambert W, Deforce D, Van Peteghem C, Van Bocxlaer J (2004) The determination of cocaine, benzoylecgonine, and cocaethylene in small volume oral fluid samples by liquid chromatography–quadrupole-time-of-flight mass spectrometry. J Anal Toxicol 28:655–659
Cognard E, Bouchonnet S, Staub C (2006) Validation of a gas chromatography–ion trap tandem mass spectrometry for simultaneous analyse of cocaine and its metabolites in saliva. J Pharm Biomed Anal 41:925–934. doi:10.1016/jpba.2006.01.041
Jufer R, Walsh SL, Cone EJ, Sampson-Cole A (2006) Effect of repeated cocaine administration on detection times in oral fluid and urine. J Anal Toxicol 30:458–462
Langel K, Engblom C, Pehrsson A, Gunnar T, Ariniemi K, Lillsunde P (2008) Drug testing in oral fluid—evaluation of sample collection devices. J Anal Toxicol 32:393–401
Peters FT, Maurer HH (2002) Bioanalytical method validation and its implications for forensic and clinical toxicology—a review. Accred Qual Assur 7:441–449. doi:10.1007/s00769-002-0516-5
Griesemer EC, Liu Y, Budd RD, Raftogianis L, Noguchi TT (1983) The determination of cocaine and its major metabolite, benzoylecgonine, in postmortem fluids and tissues by computerized gas chromatography–mass spectrometry. J Forensic Sci 28:894–900
Chinn DM, Crouch DJ, Peat MA, Finkle BS, Jennison TA (1980) Gas chromatography–chemical ionization mass spectrometry of cocaine and its metabolites in biological fluids. J Anal Toxicol 4:37–42
Needleman SB, Goodin K (1991) Liquid–liquid extraction systems for THC-COOH and benzoylecgonine. J Anal Toxicol 15:179–191
Jatlow P (1988) Cocaine: analysis, pharmacokinetics, and metabolic disposition. Yale J Biol Med 61:105–113
Langel K, Gunnar T, Ariniemi K, Rajamaki O, Lillsunde P (2011) A validated method for the detection and quantitation of 50 drugs of abuse and medicinal drugs in oral fluid by gas chromatography–mass spectrometry. J Chromatogr B 879:859–870. doi:10.1016/j.jchromb.2011.02.027
Acknowledgments
This work was financially supported by TREN-05-PF6TR-S07. 61320-518404-DRUID. The authors thank to Pirjo Lillsunde, Kaarina Langel, Kari Ariniemi, and Teemu Gunnar (National Institute for Health and Welfare, Helsinki, Finland) for their help and advice in adaptation of the LLE and GC–MS analysis system to our laboratory. The authors also thank Tünde Benkő and Edit Kopasz for technical assistance.
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Institóris, L., Angyal, V., Árok, Z. et al. A simple quantitation method for benzoylecgonine from oral fluid, blood, and urine samples used for determining 22 illicit and licit drugs by GC–MS with liquid–liquid extraction. Forensic Toxicol 30, 59–65 (2012). https://doi.org/10.1007/s11419-011-0128-z
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s11419-011-0128-z