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Pipette tip solid-phase extraction and gas chromatography - mass spectrometry for the determination of methamphetamine and amphetamine in human whole blood.
Anal Bioanal Chem. 2007 Sep; 389(2):563-70.AB

Abstract

Methamphetamine and amphetamine were extracted from human whole blood samples using pipette tip solid-phase extraction (SPE) with MonoTip C(18) tips, on which C(18)-bonded monolithic silica gel was fixed. Human whole blood (0.1 mL) containing methamphetamine and amphetamine, with N-methylbenzylamine as an internal standard, was mixed with 0.4 mL of distilled water and 50 microL of 5 M sodium hydroxide solution. After centrifugation, the supernatant was extracted to the C(18) phase of the tip (pipette tip volume, 200 microL) by 25 repeated aspirating/dispensing cycles using a manual micropipettor. Analytes retained in the C(18) phase were eluted with methanol by five repeated aspirating/dispensing cycles. After derivatization with trifluoroacetic anhydride, analytes were measured by gas chromatography - mass spectrometry with selected ion monitoring in the positive-ion electron impact mode. Recoveries of methamphetamine and amphetamine spiked into whole blood were more than 87.6 and 81.7%, respectively. Regression equations for methamphetamine and amphetamine showed excellent linearity in the range of 0.5-100 ng/0.1 mL. The limits of detection for methamphetamine and amphetamine were 0.15 and 0.11 ng/0.1 mL, respectively. Intra- and interday coefficients of variation for both stimulants were not greater than 9.6 and 13.8%, respectively. The determination of methamphetamine and amphetamine in autopsy whole blood samples is presented, and was shown to validate the present methodology.

Authors+Show Affiliations

Department of Legal Medicine, Showa University School of Medicine, 1-5-8 Hatanodai, Tokyo 142-8555, Japan.No affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

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

Language

eng

PubMed ID

17641881

Citation

Hasegawa, Chika, et al. "Pipette Tip Solid-phase Extraction and Gas Chromatography - Mass Spectrometry for the Determination of Methamphetamine and Amphetamine in Human Whole Blood." Analytical and Bioanalytical Chemistry, vol. 389, no. 2, 2007, pp. 563-70.
Hasegawa C, Kumazawa T, Lee XP, et al. Pipette tip solid-phase extraction and gas chromatography - mass spectrometry for the determination of methamphetamine and amphetamine in human whole blood. Anal Bioanal Chem. 2007;389(2):563-70.
Hasegawa, C., Kumazawa, T., Lee, X. P., Marumo, A., Shinmen, N., Seno, H., & Sato, K. (2007). Pipette tip solid-phase extraction and gas chromatography - mass spectrometry for the determination of methamphetamine and amphetamine in human whole blood. Analytical and Bioanalytical Chemistry, 389(2), 563-70.
Hasegawa C, et al. Pipette Tip Solid-phase Extraction and Gas Chromatography - Mass Spectrometry for the Determination of Methamphetamine and Amphetamine in Human Whole Blood. Anal Bioanal Chem. 2007;389(2):563-70. PubMed PMID: 17641881.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Pipette tip solid-phase extraction and gas chromatography - mass spectrometry for the determination of methamphetamine and amphetamine in human whole blood. AU - Hasegawa,Chika, AU - Kumazawa,Takeshi, AU - Lee,Xiao-Pen, AU - Marumo,Akemi, AU - Shinmen,Natsuko, AU - Seno,Hiroshi, AU - Sato,Keizo, Y1 - 2007/07/20/ PY - 2007/04/11/received PY - 2007/06/21/accepted PY - 2007/06/19/revised PY - 2007/7/21/pubmed PY - 2007/12/13/medline PY - 2007/7/21/entrez SP - 563 EP - 70 JF - Analytical and bioanalytical chemistry JO - Anal Bioanal Chem VL - 389 IS - 2 N2 - Methamphetamine and amphetamine were extracted from human whole blood samples using pipette tip solid-phase extraction (SPE) with MonoTip C(18) tips, on which C(18)-bonded monolithic silica gel was fixed. Human whole blood (0.1 mL) containing methamphetamine and amphetamine, with N-methylbenzylamine as an internal standard, was mixed with 0.4 mL of distilled water and 50 microL of 5 M sodium hydroxide solution. After centrifugation, the supernatant was extracted to the C(18) phase of the tip (pipette tip volume, 200 microL) by 25 repeated aspirating/dispensing cycles using a manual micropipettor. Analytes retained in the C(18) phase were eluted with methanol by five repeated aspirating/dispensing cycles. After derivatization with trifluoroacetic anhydride, analytes were measured by gas chromatography - mass spectrometry with selected ion monitoring in the positive-ion electron impact mode. Recoveries of methamphetamine and amphetamine spiked into whole blood were more than 87.6 and 81.7%, respectively. Regression equations for methamphetamine and amphetamine showed excellent linearity in the range of 0.5-100 ng/0.1 mL. The limits of detection for methamphetamine and amphetamine were 0.15 and 0.11 ng/0.1 mL, respectively. Intra- and interday coefficients of variation for both stimulants were not greater than 9.6 and 13.8%, respectively. The determination of methamphetamine and amphetamine in autopsy whole blood samples is presented, and was shown to validate the present methodology. SN - 1618-2642 UR - https://www.unboundmedicine.com/medline/citation/17641881/Pipette_tip_solid_phase_extraction_and_gas_chromatography___mass_spectrometry_for_the_determination_of_methamphetamine_and_amphetamine_in_human_whole_blood_ L2 - https://dx.doi.org/10.1007/s00216-007-1460-3 DB - PRIME DP - Unbound Medicine ER -