Published: Journal of Analytical Toxicology, Volume 20, Number 5, September 1996, pp. 281-286.

Simultaneous Determination of Illicit Drugs in Human Urine by Liquid Chromatography–Mass Spectrometry
M. Tatsuno, M. Nishikawa, M. Katagi, and H. Tsuchihashi

The method for simultaneous determination and confirmation of illicit drugs (e.g., methamphetamine, amphetamine, ephedrine, methylephedrine, morphine, morphine-3-glucuronide, morphine-6-glucuronide, 6-acetylmorphine, cocaine, and benzoylecgonine) in human urine by thermospray liquid chromatography–mass spectrometry (LC–MS) was studied. The LC–MS separation was performed on a reversed phase column (L-column ODS; 150 mm ¥ 4.6-mm i.d.) using a gradient mobile phase system of 100mM ammonium acetate for 1 min then linear ramps to 100mM ammonium acetate including 40% acetonitrile at 20 min. Extraction was conducted by solid-phase extraction using a Sep-pak C₁₈ cartridge. The drugs were eluted with 2 mL of 40% acetonitrile in 100mM ammonium acetate, pH3 (adjusted with acetic acid), from the cartridge. A 50-µL volume of the eluate was injected into the LC–MS. The recoveries by this extraction were 88 to 99%. The mass spectra of methamphetamine, amphetamine, ephedrine, methylephedrine, morphine, 6-acetylmorphine, cocaine, and benzoylecgonine showed the quasi-molecular [M+H]+ ion as the base peak, whereas morphine-3-glucuronide and morphine-6-glucuronide showed [MH-glucuronide]+ ion as the base peak. The calibration graphs were linear and reproducible. Detection limits of these drugs ranged from 2 to 40 ng/mL by selected ion monitoring (SIM) mode and from 50 to 400 ng/mL by scan mode. The coefficients of variation for the analysis of these drugs ranged from 4.5 to 9.5% at a concentration of 0.4 µg/mL (n = 10).

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