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Standardization of method for the analysis of dextromethorphan in urine.
Forensic Sci Int. 2006 Sep 12; 161(2-3):198-201.FS

Abstract

Dextromethorphan (DMP), an antitussive, is one of the most popular drugs among the younger generation in Korea. It usually is taken for its hallucinogenic properties and overdoses have been responsible for the fatalities that have been reported frequently. To control the abuse of DMP, the authorities restricted its use through classifying it as a controlled drug on October 2003. The purpose of this study is to provide a standard method for the analysis of DMP and its main metabolite, dextrorphan (DTP) in biological specimens. At first we established a standard operating procedure (SOP) for DMP/DTP in urine, and a method validation was performed. We also quantified DMP from 16 drug abuser's urine samples all of which were positive in the screening test for DMP. For the detection of DMP/DTP, urine samples were adjusted with 6N NaOH (pH 11) and extracted with ethylacetate. Thin layer chromatography was used as the screening test, and the final identification for DMP/DTP was used by GC/MS. The ions (m/z 271 for DMP, m/z 257 for DTP and m/z 86 for lidocaine as internal standard) were extracted from the full scan mass spectrum and were used for quantification. The selectivity, linearity of calibration, accuracy, within- and between day precision, limit of detection and quantification, recovery and stability were examined as parts of the method validation. Extracted calibration curves were linear from 100 to 2000 ng/mL for DMP and DTP with correlation coefficients better than 0.999. Limit detection was 50 ng/mL for DMP and DTP. Within-run precision (%CV) for DMP and DTP at three different concentrations (100, 500 and 1000 ng/mL) was 6.10-18.85%, and between-run precision was 1.70-7.86% for DMP and DTP. Absolute recovery for DMP and DTP was 57-74%, and relative recovery (extraction efficiency) was 80-89%. For 16 drug abuser's urine samples, the concentrations of DMP and DTP were 0.16-52.63 and 0.41-23.75 microg/mL, respectively. Method validation is an important requirement in the practice of chemical analysis, and it will be particularly useful in verifying the reliability of analytical results in the field of forensic science.

Authors+Show Affiliations

Narcotics Analysis Section, National Institute of Scientific Investigation, Yangcheon-gu, Seoul, Republic of Korea. emkim@nisi.go.krNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article
Validation Study

Language

eng

PubMed ID

16837153

Citation

Kim, Eun-Mi, et al. "Standardization of Method for the Analysis of Dextromethorphan in Urine." Forensic Science International, vol. 161, no. 2-3, 2006, pp. 198-201.
Kim EM, Lee JS, Park MJ, et al. Standardization of method for the analysis of dextromethorphan in urine. Forensic Sci Int. 2006;161(2-3):198-201.
Kim, E. M., Lee, J. S., Park, M. J., Choi, S. K., Lim, M. A., & Chung, H. S. (2006). Standardization of method for the analysis of dextromethorphan in urine. Forensic Science International, 161(2-3), 198-201.
Kim EM, et al. Standardization of Method for the Analysis of Dextromethorphan in Urine. Forensic Sci Int. 2006 Sep 12;161(2-3):198-201. PubMed PMID: 16837153.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Standardization of method for the analysis of dextromethorphan in urine. AU - Kim,Eun-Mi, AU - Lee,Ju-Seon, AU - Park,Mee-Jung, AU - Choi,Sang-Kil, AU - Lim,Mi-Ae, AU - Chung,Hee-Sun, Y1 - 2006/07/11/ PY - 2005/11/27/received PY - 2005/12/28/revised PY - 2005/12/28/accepted PY - 2006/7/14/pubmed PY - 2006/11/14/medline PY - 2006/7/14/entrez SP - 198 EP - 201 JF - Forensic science international JO - Forensic Sci Int VL - 161 IS - 2-3 N2 - Dextromethorphan (DMP), an antitussive, is one of the most popular drugs among the younger generation in Korea. It usually is taken for its hallucinogenic properties and overdoses have been responsible for the fatalities that have been reported frequently. To control the abuse of DMP, the authorities restricted its use through classifying it as a controlled drug on October 2003. The purpose of this study is to provide a standard method for the analysis of DMP and its main metabolite, dextrorphan (DTP) in biological specimens. At first we established a standard operating procedure (SOP) for DMP/DTP in urine, and a method validation was performed. We also quantified DMP from 16 drug abuser's urine samples all of which were positive in the screening test for DMP. For the detection of DMP/DTP, urine samples were adjusted with 6N NaOH (pH 11) and extracted with ethylacetate. Thin layer chromatography was used as the screening test, and the final identification for DMP/DTP was used by GC/MS. The ions (m/z 271 for DMP, m/z 257 for DTP and m/z 86 for lidocaine as internal standard) were extracted from the full scan mass spectrum and were used for quantification. The selectivity, linearity of calibration, accuracy, within- and between day precision, limit of detection and quantification, recovery and stability were examined as parts of the method validation. Extracted calibration curves were linear from 100 to 2000 ng/mL for DMP and DTP with correlation coefficients better than 0.999. Limit detection was 50 ng/mL for DMP and DTP. Within-run precision (%CV) for DMP and DTP at three different concentrations (100, 500 and 1000 ng/mL) was 6.10-18.85%, and between-run precision was 1.70-7.86% for DMP and DTP. Absolute recovery for DMP and DTP was 57-74%, and relative recovery (extraction efficiency) was 80-89%. For 16 drug abuser's urine samples, the concentrations of DMP and DTP were 0.16-52.63 and 0.41-23.75 microg/mL, respectively. Method validation is an important requirement in the practice of chemical analysis, and it will be particularly useful in verifying the reliability of analytical results in the field of forensic science. SN - 0379-0738 UR - https://www.unboundmedicine.com/medline/citation/16837153/Standardization_of_method_for_the_analysis_of_dextromethorphan_in_urine_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0379-0738(06)00363-X DB - PRIME DP - Unbound Medicine ER -