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Analysis of ketamine and norketamine in urine by automatic solid-phase extraction (SPE) and positive ion chemical ionization-gas chromatography-mass spectrometry (PCI-GC-MS).
Forensic Sci Int. 2008 Jan 30; 174(2-3):197-202.FS

Abstract

Ketamine (KT) is widely abused for hallucination and also misused as a "date-rape" drug in recent years. An analytical method using positive ion chemical ionization-gas chromatography-mass spectrometry (PCI-GC-MS) with an automatic solid-phase extraction (SPE) apparatus was studied for the determination of KT and its major metabolite, norketamine (NK), in urine. Six ketamine suspected urine samples were provided by the police. For the research of KT metabolism, KT was administered to SD rats by i.p. at a single dose of 5, 10 and 20mg/kg, respectively, and urine samples were collected 24, 48 and 72 h after administration. For the detection of KT and NK, urine samples were extracted on an automatic SPE apparatus (RapidTrace, Zymark) with mixed mode type cartridge, Drug-Clean (200 mg, Alltech). The identification of KT and NK was by PCI-GC-MS. m/z238 (M+1), 220 for KT, m/z 224 (M+1), 207 for NK and m/z307 (M+1) for Cocaine-D(3) as internal standard were extracted from the full-scan mass spectrum and the underlined ions were used for quantitation. Extracted calibration curves were linear from 50 to 1000 ng/mL for KT and NK with correlation coefficients exceeding 0.99. The limit of detection (LOD) was 25 ng/mL for KT and NK. The limit of quantitation (LOQ) was 50 ng/mL for KT and NK. The recoveries of KT and NK at three different concentrations (86, 430 and 860 ng/mL) were 53.1 to 79.7% and 45.7 to 83.0%, respectively. The intra- and inter-day run precisions (CV) for KT and NK were less than 15.0%, and the accuracies (bias) for KT and NK were also less than 15% at the three different concentration levels (86, 430 and 860 ng/mL). The analytical method was also applied to real six KT suspected urine specimens and KT administered rat urines, and the concentrations of KT and NK were determined. Dehydronorketamine (DHNK) was also confirmed in these urine samples, however the concentration of DHNK was not calculated. SPE is simple, and needs less organic solvent than liquid-liquid extraction (LLE), and PCI-GC-MS can offer both qualitative and quantitative information for urinalysis of KT in forensic analysis.

Authors+Show Affiliations

Narcotics Analysis Section, National Institute of Scientific Investigation, 331-1 Shinwol 7-dong, Yangcheon-gu, Seoul 158-707, Republic of Korea. emkim@nisi.go.krNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article

Language

eng

PubMed ID

17553643

Citation

Kim, Eun-mi, et al. "Analysis of Ketamine and Norketamine in Urine By Automatic Solid-phase Extraction (SPE) and Positive Ion Chemical Ionization-gas Chromatography-mass Spectrometry (PCI-GC-MS)." Forensic Science International, vol. 174, no. 2-3, 2008, pp. 197-202.
Kim EM, Lee JS, Choi SK, et al. Analysis of ketamine and norketamine in urine by automatic solid-phase extraction (SPE) and positive ion chemical ionization-gas chromatography-mass spectrometry (PCI-GC-MS). Forensic Sci Int. 2008;174(2-3):197-202.
Kim, E. M., Lee, J. S., Choi, S. K., Lim, M. A., & Chung, H. S. (2008). Analysis of ketamine and norketamine in urine by automatic solid-phase extraction (SPE) and positive ion chemical ionization-gas chromatography-mass spectrometry (PCI-GC-MS). Forensic Science International, 174(2-3), 197-202.
Kim EM, et al. Analysis of Ketamine and Norketamine in Urine By Automatic Solid-phase Extraction (SPE) and Positive Ion Chemical Ionization-gas Chromatography-mass Spectrometry (PCI-GC-MS). Forensic Sci Int. 2008 Jan 30;174(2-3):197-202. PubMed PMID: 17553643.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Analysis of ketamine and norketamine in urine by automatic solid-phase extraction (SPE) and positive ion chemical ionization-gas chromatography-mass spectrometry (PCI-GC-MS). AU - Kim,Eun-mi, AU - Lee,Ju-seon, AU - Choi,Sang-kil, AU - Lim,Mi-ae, AU - Chung,Hee-sun, Y1 - 2007/06/05/ PY - 2007/04/16/received PY - 2007/04/23/accepted PY - 2007/6/8/pubmed PY - 2008/2/6/medline PY - 2007/6/8/entrez SP - 197 EP - 202 JF - Forensic science international JO - Forensic Sci. Int. VL - 174 IS - 2-3 N2 - Ketamine (KT) is widely abused for hallucination and also misused as a "date-rape" drug in recent years. An analytical method using positive ion chemical ionization-gas chromatography-mass spectrometry (PCI-GC-MS) with an automatic solid-phase extraction (SPE) apparatus was studied for the determination of KT and its major metabolite, norketamine (NK), in urine. Six ketamine suspected urine samples were provided by the police. For the research of KT metabolism, KT was administered to SD rats by i.p. at a single dose of 5, 10 and 20mg/kg, respectively, and urine samples were collected 24, 48 and 72 h after administration. For the detection of KT and NK, urine samples were extracted on an automatic SPE apparatus (RapidTrace, Zymark) with mixed mode type cartridge, Drug-Clean (200 mg, Alltech). The identification of KT and NK was by PCI-GC-MS. m/z238 (M+1), 220 for KT, m/z 224 (M+1), 207 for NK and m/z307 (M+1) for Cocaine-D(3) as internal standard were extracted from the full-scan mass spectrum and the underlined ions were used for quantitation. Extracted calibration curves were linear from 50 to 1000 ng/mL for KT and NK with correlation coefficients exceeding 0.99. The limit of detection (LOD) was 25 ng/mL for KT and NK. The limit of quantitation (LOQ) was 50 ng/mL for KT and NK. The recoveries of KT and NK at three different concentrations (86, 430 and 860 ng/mL) were 53.1 to 79.7% and 45.7 to 83.0%, respectively. The intra- and inter-day run precisions (CV) for KT and NK were less than 15.0%, and the accuracies (bias) for KT and NK were also less than 15% at the three different concentration levels (86, 430 and 860 ng/mL). The analytical method was also applied to real six KT suspected urine specimens and KT administered rat urines, and the concentrations of KT and NK were determined. Dehydronorketamine (DHNK) was also confirmed in these urine samples, however the concentration of DHNK was not calculated. SPE is simple, and needs less organic solvent than liquid-liquid extraction (LLE), and PCI-GC-MS can offer both qualitative and quantitative information for urinalysis of KT in forensic analysis. SN - 1872-6283 UR - https://www.unboundmedicine.com/medline/citation/17553643/Analysis_of_ketamine_and_norketamine_in_urine_by_automatic_solid_phase_extraction__SPE__and_positive_ion_chemical_ionization_gas_chromatography_mass_spectrometry__PCI_GC_MS__ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0379-0738(07)00453-7 DB - PRIME DP - Unbound Medicine ER -