A systematic evaluation that compares the recoveries of methamphetamine and amphetamine from spiked urine using C8, C18, strong cation exchanger (SCX), and C8-SCX mixed procedures (solid-phase extraction) is reported. Optimized experimental conditions including pH of the sample, solvent composition, and urine concentration for different solid-phase extraction sorbents were studied. The largest recoveries--greater than 86% for methamphetamine and greater than 88% for amphetamine--were achieved with a mixed adsorbent (C8-SCX) and mixed elution solvent CH2Cl2-i-propanol-NH4OH (78:20:2) at pH 6. The concentration of the urine matrix did not affect the extraction efficiency. The detection limits of methamphetamine and amphetamine in urine were obtained at 0.03 and 0.07 micrograms/mL, respectively, using gas chromatographic-mass spectrometric analysis operated in the electron impact mode.
Optimized experimental procedures including time of extraction, extraction solvent in Soxhlet extraction technique were sought for detection of trace ethion residues in soil. The largest recoveries over 96% were achieved with a 1:1 mixture of methanol and acetone as extraction solvent for three hours. In comparing EI, CI, EI‐CAD, and PCI‐CAD modes of a four sector mass spectrometry for detection ethion, it was shown the best monitoring mode to be EI monitoring of the M+ of ethion, m/z 384, which fragments to give the m/z 231 product ion. The limit of detection obtained was 170 pg/g in soil.
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