Abstract
Methamphetamine and amphetamine were extracted from human whole blood samples using pipette tip solid-phase extraction (SPE) with MonoTip C18 tips, on which C18-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 μL of 5 M sodium hydroxide solution. After centrifugation, the supernatant was extracted to the C18 phase of the tip (pipette tip volume, 200 μL) by 25 repeated aspirating/dispensing cycles using a manual micropipettor. Analytes retained in the C18 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.
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Bar AM, Panenka WJ, MacEwan W, Thornton AE, Lang DJ, Honer WG, Lecomte T (2006) J Psychiatr Neurosci 31:301–313
Takayasu T, Ohshima T, Nishigami J, Kondo T, Nagano T (1995) J Clin Forensic Med 2:25–33
Sato M, Mitsui T (1997) J Pharm Biomed Anal 16:139–145
Kumazawa T, Watanabe-Suzuki K, Seno H, Ishii A, Suzuki O (2000) Legal Med 2:181–185
Okajima K, Namera A, Yashiki M, Tsukue I, Kojima T (2001) Forensic Sci Int 116:15–22
Ishigami A, Kubo S, Gotohda T, Tokunaga I (2003) J Med Invest 50:112–116
Ago M, Ago K, Hara K, Kashimura S, Ogata M (2006) Legal Med 8:235–239
Nishida M, Yashiki M, Namera A, Kimura K (2006) J Chromatogr B 842:106–110
Lambert WE, Meyer E, De Leenheer AP (1995) J Anal Toxicol 19:73–78
Marquet P, Lacassie E, Battu C, Faubert H, Lachâtre G (1997) J Chromatogr B 700:77–82
Kupiec T, DeCicco L, Spiehler V, Sneed G, Kemp P (2002) J Anal Toxicol 26:513–518
Boatto G, Faedda MV, Pau A, Asproni B, Menconi S, Cerri R (2002) J Pharm Biomed Anal 29:1073–1080
Kumazawa T, Sato K, Seno H, Suzuki O (1993) Jpn J Legal Med (Nihon Hoigaku Zasshi) 47:129–133
Zweipfenning PGM, Wilderink AHCH, Horsthuis P, Franke J-P, de Zeeuw RA (1994) J Chromatogr A 674:87–95
Hara K, Kashimura S, Hieda Y, Kageura M (1997) J Anal Toxicol 21:54–58
Namera A, Yashiki M, Liu J, Okajima K, Hara K, Imamura T, Kojima T (2000) Forensic Sci Int 109:215–223
Nagawasa N, Yashiki M, Iwasaki Y, Hara K, Kojima T (1996) Forensic Sci Int 78:95–102
van Vliet C, Swean GM, Slangen JJ, De Boorder T, Sturmans F (1987) Int Arch Occup Environ Health 59:493–501
Fujimaki K, Lee X-P, Kumazawa T, Sato J, Sato K (2006) Forensic Toxicol 24:8–16
Pluskal MG, Bogdanova A, Lopez M, Gutierrez S, Pitt AM (2002) Proteomics 2:145–150
Keough T, Lacey MP, Youngquist RS (2002) Rapid Commun Mass Spectrom 16:1003–1015
Tannu NS, Wu J, Rao VK, Gadgil HS, Pabst MJ, Gerling IC, Raghow R (2004) Anal Biochem 327:222–232
Šalplachta J, Řehulka P, Chmelík J (2004) J Mass Spectrom 39:1395–1401
Majors RE, Shukla A (2005) Micropipette tip-based sample preparation for bioanalysis. LC–GC N Am, 1 July (see http://www.lcgcmag.com/lcgc/, cited 3 July 2007)
Palmblad M, Vogel JS (2005) J Chromatogr B 814:309–313
Li G, Hu R, Kamijo Y, Nakajima T, Aoyama T, Inoue T, Node K, Kannagi R, Kyogashima M, Hara A (2007) Anal Biochem 362:1–7
Miyazaki S, Morisato K, Ishizuka N, Minakuchi H, Shintani Y, Furuno M, Nakanishi K (2004) J Chromatogr A 1043:19–25
Hasegawa C, Kumazawa T, Lee X-P, Fujishiro M, Kuriki A, Marumo A, Seno H, Sato K (2006) Rapid Commun Mass Spectrom 20:537–543
Kumazawa T, Hasegawa C, Lee X-P, Marumo A, Shimmen N, Ishii A, Seno H, Sato K (2006) Talanta 70:474–478
Kumazawa T, Hasegawa C, Lee X-P, Hara K, Seno H, Suzuki O, Sato K (2007) J Pharm Biomed Anal 44:602–607
Shen JX, Tama CI, Hayes RN (2006) J Chromatogr B 843:275–282
Campíns-Falcó P, Sevillano-Cabeza A, Molíns-Legua C, Kohlmann M (1996) J Chromatogr B 687:239–246
Margalho C, de Boer D, Gallardo E, Barroso M, Vieira DN (2005) J Anal Toxicol 29:309–313
Sánchez de la Torre C, Martínez MA, Almarza E (2005) Forensic Sci Int 155:193–204
Huang Z, Zhang S (2003) J Chromatogr B 792:241–247
Suzuki O, Kumazawa T, Seno H, Hattori H (1989) Med Sci Law 29:242–247
Marumo A, Kumazawa T, Lee X-P, Fujimaki K, Kuriki A, Hasegawa C, Sato K, Seno H, Suzuki O (2005) J AOAC Int 88:1655–1660
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This study was supported in part by a grant-in-aid from the Ministry of Education, Science, Sports and Culture of Japan.
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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 389, 563–570 (2007). https://doi.org/10.1007/s00216-007-1460-3
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DOI: https://doi.org/10.1007/s00216-007-1460-3