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A sensitive semi-micro column HPLC method with peroxyoxalate chemiluminescence detection and column switching for determination of MDMA-related compounds in hair

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Abstract

A sensitive semi-micro column HPLC method with peroxyoxalate chemiluminescence (POCL) detection and column switching has been developed for simultaneous determination of 3,4-methylenedioxymethamphetamine (MDMA) and related compounds, for example 3,4-methylenedioxyamphetamine, methamphetamine, and amphetamine, in hair. After digestion of the hair with 1 mol L−1 sodium hydroxide the compounds were extracted with n-heptane and derivatized with 4-(N,N-dimethylaminosulfonyl)-7-fluoro-2,1,3-benzoxadiazole. A mixture of hydrogen peroxide and bis(2,4,5-trichloro-6-carbopentoxyphenyl)oxalate in acetonitrile was used as post-column CL reagent. Calibration plots showed linearity was good (r = 0.999); detection limits were 0.02–0.16 ng mg−1 hair at a signal-to-noise ratio of 3. The precision of the method, as RSD (n = 5), in intra-day and inter-day assays was better than 5.0 and 6.9%, respectively. The proposed method was sufficiently sensitive to detect low ng mg−1 levels of MDMA and related compounds in hair, and could be used for quantification of the compounds in hair samples from patients treated in a chemical dependency unit.

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References

  1. Nakashima K (2005) J Health Sci 51(3):272–277

    Article  CAS  Google Scholar 

  2. Tagliaro F, Battisti DZ, Groppi A, Nakahara Y, Scarcella D, Valentini R, Marigo M (1999) J Chromatogr B 723:195–202

    CAS  Google Scholar 

  3. Freese ET, Miotto K, Reback JC (2002) J Subst Abuse Treat 23:151–156

    Article  Google Scholar 

  4. Oesterheld RJ, Armstrong CS, Cozza LK (2004) Psychosomatics 45(1):84–87

    Article  CAS  Google Scholar 

  5. Gowing RL, Henry-Edwards MS, Irvine JR, Ali LR (2002) Drug Alcohol Rev 21:53–63

    Article  Google Scholar 

  6. Kalasinsky SK, Hugel J, Kish JS (2004) J Forensic Sci 49(5):1106–1112

    Article  Google Scholar 

  7. Gambelunghe C, Rossi R, Ferranti C, Rossi R, Bacci M (2005) J Appl Toxicol 25:205–211

    Article  CAS  Google Scholar 

  8. Wada M, Nakashima K (2006) Anal Bioanal Chem 385:413–415

    Article  CAS  Google Scholar 

  9. Nakashima K, Kaddoumi A, Ishida Y, Itoh T, Taki K (2003) Biomed Chromatogr 17:471–476

    Article  CAS  Google Scholar 

  10. Kaddoumi A, Wada M, Nakashima NM, Nakashima K (2004) Forensic Sci Int 146:39–46

    Article  CAS  Google Scholar 

  11. Nakamura S, Tomita M, Wada M, Chung H, Kuroda N, Nakashima K (2006) Biomed Chromatogr 20:622–627

    Article  CAS  Google Scholar 

  12. Nakashima K, Suetsugu K, Yoshida K, Akiyama S (1992) Biomed Chromatogr 6:149–154

    Article  CAS  Google Scholar 

  13. Wada M, Nakamura S, Tomita M, Nakashima NM, Nakashima K (2005) Luminescence 20:210–215

    Article  CAS  Google Scholar 

  14. Nagai N (1893) Yakugaku Zasshi 13:901–933

    Google Scholar 

  15. Pujadas M, Pichini S, Poudevida S, Menoyo E, Zuccaro P, Farré M, de la Torre R (2003) J Chromatogr B 798:249–255

    Article  CAS  Google Scholar 

  16. Skender L, Karaèic V, Brèic I, Bagariæ A (2002) Forensic Sci Int 125:120–126

    Article  CAS  Google Scholar 

  17. Han E, Yang W, Lee J, Park Y, Kim E, Lim M, Chung H (2005) Forensic Sci Int 152:73–77

    Article  CAS  Google Scholar 

  18. Takayama N, Tanaka S, Hayakawa K (1997) Biomed Chromatogr 11:25–28

    Article  CAS  Google Scholar 

  19. Miki A, Katagi M, Tsuchihashi H (2003) J Anal Toxicol 27:95–102

    CAS  Google Scholar 

  20. Kronstrand R, Nyström I, Strandberg J, Druid H (2004) Forensic Sci Int 145:183–190

    Article  CAS  Google Scholar 

  21. Villamor JL, Bermejo AM, Fernandez P, Tabernero MJ (2005) J Anal Toxicol 29:135–139

    CAS  Google Scholar 

  22. Han E, Park Y, Yang W, Lee J, Lee S, Kim E, Lim M, Chung H (2006) Forensic Sci Int 161:124–129

    Article  CAS  Google Scholar 

Download references

Acknowledgments

The authors gratefully acknowledge financial support from Ministry of Health, Labor and Welfare of Japan.

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Authors and Affiliations

  1. Department of Clinical Pharmacy, Graduate School of Biomedical Sciences, Nagasaki University, 1-14 Bunkyo-machi, Nagasaki, 852-8521, Japan

    Shinichi Nakamura, Mitsuhiro Wada, Naotaka Kuroda & Kenichiro Nakashima

  2. Mississippi State Hospital, Whitfield, MS, 39193, USA

    Brian L. Crabtree, Patricia M. Reeves & John H. Montgomery

  3. The University of Mississippi Medical Center, 2500 North State Street, Jackson, MS, 39216-4505, USA

    Brian L. Crabtree & H. Joseph Byrd

  4. Lumica Corporation, 65 Itogaura, Koga, Fukuoka, 811-3136, Japan

    Shiro Harada

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  1. Shinichi Nakamura
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  2. Mitsuhiro Wada
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  3. Brian L. Crabtree
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  4. Patricia M. Reeves
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  5. John H. Montgomery
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  6. H. Joseph Byrd
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  7. Shiro Harada
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  8. Naotaka Kuroda
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  9. Kenichiro Nakashima
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Correspondence to Kenichiro Nakashima.

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Nakamura, S., Wada, M., Crabtree, B.L. et al. A sensitive semi-micro column HPLC method with peroxyoxalate chemiluminescence detection and column switching for determination of MDMA-related compounds in hair. Anal Bioanal Chem 387, 1983–1990 (2007). https://doi.org/10.1007/s00216-006-0915-2

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  • DOI: https://doi.org/10.1007/s00216-006-0915-2

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