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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. 2005 Jun; 40(6):739-53.JM

Abstract

An analytical procedure was developed for the simultaneous sensitive identification, screening and quantitation of 30 drugs of abuse using 250 microl of human oral fluid. The method employs sequential mixed-mode solid-phase extraction (SPE), optimized derivative formation and long-column fast gas chromatography/electron impact mass spectrometry (GC/EI-MS). After sequential SPE elution, the most sensitive and stable derivatives were formed by taking careful account of the characteristics of the active functional groups and possible steric hindrances affecting derivatization chemistry. Amphetamine-type stimulant drugs were acylated with heptafluorobutyric anhydride, benzodiazepines and Delta(9)-tetrahydrocannabinol were silylated with N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide and benzoylecgonine, codeine, ethylmorphine, 6-monoacetylmorphine, morphine, pholcodine, buprenorphine and norbuprenorphine with N-methyl-N-(trimethylsilyl)trifluoroacetamide. In addition, the following analytes were included: methadone, cocaine, alprazolam, midazolam, fentanyl and zolpidem. In GC separation, fast temperature ramping and high carrier gas flow-rate combined with long 30 m columns of i.d. 0.32 mm offered a reduction in analysis time and sharp peak shapes while still maintaining sufficient resolution and high sample capacity. Validated parameters including selectivity, linearity, accuracy, intra- and inter-day precision, extraction efficiency and limit of quantitation were all within required limits. In contrast to previously published methods, this single procedure is suitable for the simultaneous toxicological determination of the most common illicit drugs and benzodiazepines, and also zolpidem, in a small amount of oral fluid.

Authors+Show Affiliations

National Public Health Institute, Drug Research Unit, Mannerheimintie 166, 00300 Helsinki, Finland. teemu.gunnar@ktl.fiNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't
Validation Study

Language

eng

PubMed ID

15806585

Citation

Gunnar, Teemu, et al. "Validated Toxicological Determination of 30 Drugs of Abuse as Optimized Derivatives in Oral Fluid By Long Column Fast Gas Chromatography/electron Impact Mass Spectrometry." Journal of Mass Spectrometry : JMS, vol. 40, no. 6, 2005, pp. 739-53.
Gunnar T, Ariniemi K, Lillsunde P. 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. 2005;40(6):739-53.
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. Journal of Mass Spectrometry : JMS, 40(6), 739-53.
Gunnar T, Ariniemi K, Lillsunde P. 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. 2005;40(6):739-53. PubMed PMID: 15806585.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Validated toxicological determination of 30 drugs of abuse as optimized derivatives in oral fluid by long column fast gas chromatography/electron impact mass spectrometry. AU - Gunnar,Teemu, AU - Ariniemi,Kari, AU - Lillsunde,Pirjo, PY - 2005/4/5/pubmed PY - 2005/8/5/medline PY - 2005/4/5/entrez SP - 739 EP - 53 JF - Journal of mass spectrometry : JMS JO - J Mass Spectrom VL - 40 IS - 6 N2 - An analytical procedure was developed for the simultaneous sensitive identification, screening and quantitation of 30 drugs of abuse using 250 microl of human oral fluid. The method employs sequential mixed-mode solid-phase extraction (SPE), optimized derivative formation and long-column fast gas chromatography/electron impact mass spectrometry (GC/EI-MS). After sequential SPE elution, the most sensitive and stable derivatives were formed by taking careful account of the characteristics of the active functional groups and possible steric hindrances affecting derivatization chemistry. Amphetamine-type stimulant drugs were acylated with heptafluorobutyric anhydride, benzodiazepines and Delta(9)-tetrahydrocannabinol were silylated with N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide and benzoylecgonine, codeine, ethylmorphine, 6-monoacetylmorphine, morphine, pholcodine, buprenorphine and norbuprenorphine with N-methyl-N-(trimethylsilyl)trifluoroacetamide. In addition, the following analytes were included: methadone, cocaine, alprazolam, midazolam, fentanyl and zolpidem. In GC separation, fast temperature ramping and high carrier gas flow-rate combined with long 30 m columns of i.d. 0.32 mm offered a reduction in analysis time and sharp peak shapes while still maintaining sufficient resolution and high sample capacity. Validated parameters including selectivity, linearity, accuracy, intra- and inter-day precision, extraction efficiency and limit of quantitation were all within required limits. In contrast to previously published methods, this single procedure is suitable for the simultaneous toxicological determination of the most common illicit drugs and benzodiazepines, and also zolpidem, in a small amount of oral fluid. SN - 1076-5174 UR - https://www.unboundmedicine.com/medline/citation/15806585/Validated_toxicological_determination_of_30_drugs_of_abuse_as_optimized_derivatives_in_oral_fluid_by_long_column_fast_gas_chromatography/electron_impact_mass_spectrometry_ L2 - https://doi.org/10.1002/jms.846 DB - PRIME DP - Unbound Medicine ER -