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Rapid identification and quantification of methamphetamine and amphetamine in hair by gas chromatography/mass spectrometry coupled with micropulverized extraction, aqueous acetylation and microextraction by packed sorbent.
J Chromatogr A. 2009 May 01; 1216(18):4063-70.JC

Abstract

We developed a rapid identification and quantification method for the toxicological analysis of methamphetamine and amphetamine in human hair by gas chromatography/mass spectrometry coupled with a novel combination of micropulverized extraction, aqueous acetylation and microextraction by packed sorbent (MEPS) named MiAMi-GC/MS. A washed hair sample (1-5 mg) was micropulverized for 5 min in a 2 mL plastic tube with 250 microL of water. An anion-exchange sorbent was added to adsorb anionic interferences. After removing the residue with a membrane-filter unit, sodium carbonate and acetic anhydride was admixed in turn. Acetylation was completed in approximately 20 min at room temperature. The acetylated analytes in the reaction liquid were concentrated to an octadecylsilica sorbent packed in the needle of a syringe by a CombiPAL autosampler. Elution was carried out with 50 microL of methanol, and the entire eluate injected into a gas chromatograph using a programmable temperature vaporizing (PTV) technique. The time required for sample preparation and GC/MS analysis was approximately 1 h from a washed hair sample, and an evaporation process was not required. Ranges for quantification were 0.20-50 (ng/mg) each for methamphetamine and amphetamine using 1 mg of hair. Accuracy and relative standard deviation (RSD) were evaluated intraday and interday at three concentrations, and the results were within the limit of a guidance issued by U.S. Food and Drug Administration. For identification, full-scan mass spectra of methamphetamine and amphetamine were obtained using 5 mg of fortified hair samples at 0.2 ng/mg. The extraction device of MEPS was durable for at least 300 extractions, whereas the liner of the gas chromatograph should be replaced after 20-30 times use. The carry over was estimated to be about 1-2%. This sample-preparation method coupled with GC/MS is fast and labor-saving in comparison with conventional methods.

Authors+Show Affiliations

National Research Institute of Police Science, 6-3-1 Kashiwanoha, Kashiwa, Chiba 277-0882, Japan. miyaguchi@nrips.go.jpNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Evaluation Study
Journal Article

Language

eng

PubMed ID

19286186

Citation

Miyaguchi, Hajime, et al. "Rapid Identification and Quantification of Methamphetamine and Amphetamine in Hair By Gas Chromatography/mass Spectrometry Coupled With Micropulverized Extraction, Aqueous Acetylation and Microextraction By Packed Sorbent." Journal of Chromatography. A, vol. 1216, no. 18, 2009, pp. 4063-70.
Miyaguchi H, Iwata YT, Kanamori T, et al. Rapid identification and quantification of methamphetamine and amphetamine in hair by gas chromatography/mass spectrometry coupled with micropulverized extraction, aqueous acetylation and microextraction by packed sorbent. J Chromatogr A. 2009;1216(18):4063-70.
Miyaguchi, H., Iwata, Y. T., Kanamori, T., Tsujikawa, K., Kuwayama, K., & Inoue, H. (2009). Rapid identification and quantification of methamphetamine and amphetamine in hair by gas chromatography/mass spectrometry coupled with micropulverized extraction, aqueous acetylation and microextraction by packed sorbent. Journal of Chromatography. A, 1216(18), 4063-70. https://doi.org/10.1016/j.chroma.2009.02.093
Miyaguchi H, et al. Rapid Identification and Quantification of Methamphetamine and Amphetamine in Hair By Gas Chromatography/mass Spectrometry Coupled With Micropulverized Extraction, Aqueous Acetylation and Microextraction By Packed Sorbent. J Chromatogr A. 2009 May 1;1216(18):4063-70. PubMed PMID: 19286186.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Rapid identification and quantification of methamphetamine and amphetamine in hair by gas chromatography/mass spectrometry coupled with micropulverized extraction, aqueous acetylation and microextraction by packed sorbent. AU - Miyaguchi,Hajime, AU - Iwata,Yuko T, AU - Kanamori,Tatsuyuki, AU - Tsujikawa,Kenji, AU - Kuwayama,Kenji, AU - Inoue,Hiroyuki, Y1 - 2009/03/06/ PY - 2008/11/19/received PY - 2009/02/02/revised PY - 2009/02/27/accepted PY - 2009/3/17/entrez PY - 2009/3/17/pubmed PY - 2009/6/24/medline SP - 4063 EP - 70 JF - Journal of chromatography. A JO - J Chromatogr A VL - 1216 IS - 18 N2 - We developed a rapid identification and quantification method for the toxicological analysis of methamphetamine and amphetamine in human hair by gas chromatography/mass spectrometry coupled with a novel combination of micropulverized extraction, aqueous acetylation and microextraction by packed sorbent (MEPS) named MiAMi-GC/MS. A washed hair sample (1-5 mg) was micropulverized for 5 min in a 2 mL plastic tube with 250 microL of water. An anion-exchange sorbent was added to adsorb anionic interferences. After removing the residue with a membrane-filter unit, sodium carbonate and acetic anhydride was admixed in turn. Acetylation was completed in approximately 20 min at room temperature. The acetylated analytes in the reaction liquid were concentrated to an octadecylsilica sorbent packed in the needle of a syringe by a CombiPAL autosampler. Elution was carried out with 50 microL of methanol, and the entire eluate injected into a gas chromatograph using a programmable temperature vaporizing (PTV) technique. The time required for sample preparation and GC/MS analysis was approximately 1 h from a washed hair sample, and an evaporation process was not required. Ranges for quantification were 0.20-50 (ng/mg) each for methamphetamine and amphetamine using 1 mg of hair. Accuracy and relative standard deviation (RSD) were evaluated intraday and interday at three concentrations, and the results were within the limit of a guidance issued by U.S. Food and Drug Administration. For identification, full-scan mass spectra of methamphetamine and amphetamine were obtained using 5 mg of fortified hair samples at 0.2 ng/mg. The extraction device of MEPS was durable for at least 300 extractions, whereas the liner of the gas chromatograph should be replaced after 20-30 times use. The carry over was estimated to be about 1-2%. This sample-preparation method coupled with GC/MS is fast and labor-saving in comparison with conventional methods. SN - 1873-3778 UR - https://www.unboundmedicine.com/medline/citation/19286186/Rapid_identification_and_quantification_of_methamphetamine_and_amphetamine_in_hair_by_gas_chromatography/mass_spectrometry_coupled_with_micropulverized_extraction_aqueous_acetylation_and_microextraction_by_packed_sorbent_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0021-9673(09)00347-1 DB - PRIME DP - Unbound Medicine ER -