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Quantitative detection of ketamine, norketamine, and dehydronorketamine in urine using chemical derivatization followed by gas chromatography-mass spectrometry.
J Chromatogr B Analyt Technol Biomed Life Sci. 2005 Jun 25; 820(2):165-73.JC

Abstract

A repeatable and highly sensitive analytical method using gas chromatography-mass spectrometry (GC-MS) in the selected ion monitoring mode (SIM) is developed for the simultaneous detection of ketamine (KT), norketamine (NK), and newly introduced dehydronorketamine (DHNK) in urine. The test specimen along with the deuterium analogues as internal standards (IS): d4-KT for KT and d4-NK for NK/DHNK, was extracted on an automatic solid-phase extraction (SPE) apparatus. The extracted eluate then was dried and derivatized with N-methyl-bis(trifluoroacetamide) (CF3CONCH3COCF3, MBTFA). Finally, the cooled derivatized solution was directly injected into the GC-MS system for analysis. The proposed process achieves high sensitivity for the detection of KT, NK, and DHNK. Correlation coefficients derived from typical calibration curves in the range of 20-2000 ng/mL are 1.000 for KT and NK, 0.999 for DHNK. The limits of detection (LODs) and limits of quantitation (LOQs) are 0.5-1.0 and 1.5-3.0, respectively. The overall method recoveries of KT, NK, and DHNK are 82.2-93.4. The intra- and inter-day run deviations are smaller than 5.0%. The analytical scheme was also applied to the determination of KT, NK, and DHNK in 20 KT suspected urine specimens, and the results reconfirm that DHNK is a main metabolite of KT.

Authors+Show Affiliations

National Bureau of Controlled Drugs, DOH, Taipei, Taiwan, ROC.No affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

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

Language

eng

PubMed ID

15899370

Citation

Huang, Min-Kun, et al. "Quantitative Detection of Ketamine, Norketamine, and Dehydronorketamine in Urine Using Chemical Derivatization Followed By Gas Chromatography-mass Spectrometry." Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, vol. 820, no. 2, 2005, pp. 165-73.
Huang MK, Liu C, Li JH, et al. Quantitative detection of ketamine, norketamine, and dehydronorketamine in urine using chemical derivatization followed by gas chromatography-mass spectrometry. J Chromatogr B Analyt Technol Biomed Life Sci. 2005;820(2):165-73.
Huang, M. K., Liu, C., Li, J. H., & Huang, S. D. (2005). Quantitative detection of ketamine, norketamine, and dehydronorketamine in urine using chemical derivatization followed by gas chromatography-mass spectrometry. Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, 820(2), 165-73.
Huang MK, et al. Quantitative Detection of Ketamine, Norketamine, and Dehydronorketamine in Urine Using Chemical Derivatization Followed By Gas Chromatography-mass Spectrometry. J Chromatogr B Analyt Technol Biomed Life Sci. 2005 Jun 25;820(2):165-73. PubMed PMID: 15899370.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Quantitative detection of ketamine, norketamine, and dehydronorketamine in urine using chemical derivatization followed by gas chromatography-mass spectrometry. AU - Huang,Min-Kun, AU - Liu,Chiareiy, AU - Li,Jih-Heng, AU - Huang,Shang-Da, Y1 - 2005/04/26/ PY - 2004/05/11/received PY - 2004/12/31/revised PY - 2005/03/01/accepted PY - 2005/5/19/pubmed PY - 2005/10/12/medline PY - 2005/5/19/entrez SP - 165 EP - 73 JF - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JO - J Chromatogr B Analyt Technol Biomed Life Sci VL - 820 IS - 2 N2 - A repeatable and highly sensitive analytical method using gas chromatography-mass spectrometry (GC-MS) in the selected ion monitoring mode (SIM) is developed for the simultaneous detection of ketamine (KT), norketamine (NK), and newly introduced dehydronorketamine (DHNK) in urine. The test specimen along with the deuterium analogues as internal standards (IS): d4-KT for KT and d4-NK for NK/DHNK, was extracted on an automatic solid-phase extraction (SPE) apparatus. The extracted eluate then was dried and derivatized with N-methyl-bis(trifluoroacetamide) (CF3CONCH3COCF3, MBTFA). Finally, the cooled derivatized solution was directly injected into the GC-MS system for analysis. The proposed process achieves high sensitivity for the detection of KT, NK, and DHNK. Correlation coefficients derived from typical calibration curves in the range of 20-2000 ng/mL are 1.000 for KT and NK, 0.999 for DHNK. The limits of detection (LODs) and limits of quantitation (LOQs) are 0.5-1.0 and 1.5-3.0, respectively. The overall method recoveries of KT, NK, and DHNK are 82.2-93.4. The intra- and inter-day run deviations are smaller than 5.0%. The analytical scheme was also applied to the determination of KT, NK, and DHNK in 20 KT suspected urine specimens, and the results reconfirm that DHNK is a main metabolite of KT. SN - 1570-0232 UR - https://www.unboundmedicine.com/medline/citation/15899370/Quantitative_detection_of_ketamine_norketamine_and_dehydronorketamine_in_urine_using_chemical_derivatization_followed_by_gas_chromatography_mass_spectrometry_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S1570-0232(05)00199-6 DB - PRIME DP - Unbound Medicine ER -