期刊
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
卷 389, 期 2, 页码 563-570出版社
SPRINGER HEIDELBERG
DOI: 10.1007/s00216-007-1460-3
关键词
solid-phase extraction (SPE); methamphetamine; amphetamine; gas chromatography; mass spectrometry
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 mu L of 5 M sodium hydroxide solution. After centrifugation, the supernatant was extracted to the C-18 phase of the tip (pipette tip volume, 200 mu L) 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.
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