Determination of amphetamines in human urine by liquid chromatography with fluorimetric detection using a solid‐phase extraction procedure

Abstract

A precise and feasible HPLC method has been developed for the analysis of amphetamine (AMPH), methamphetamine (MAMPH) and methylenedioxymethamphetamine (MDMA, ecstasy) in human urine. A chromatographic run on a C8 Genesis (150 mm x 4.6 mm, 5 microm) column maintained at 30 degrees C lasts about 17 min, using a mobile phase composed of ACN (12%) and a pH 2.5 phosphate buffer (88%) containing 0.3% triethylamine. Mirtazapine was used as the internal standard. Good linearity was found in the 100-2000 ng/mL concentration range for AMPH and MAMPH and in the 12-2000 ng/mL concentration range for MDMA. The pretreatment of urine samples was carried out by means of a careful SPE procedure on C2 cartridges. The extraction yields were very satisfactory for all analytes, with average values greater than 97%. The leading conditions allowed the determination of AMPH, MAMPH and MDMA with satisfactory precision and accuracy. The method has been successfully applied to the determination of the analytes in urine of AMPH users.

Trends in bioanalytical methods for the determination and quantification of club drugs: 2000–2010

“…In addition to UV detection or DAD as alternatives to MS as a detector for LC, a few laboratories utilize derivatization techniques to make the drugs suitable for fluorescence detection. Fluorescence detection (FD) is exploited in GHB analysis (Zacharis et al ., 2008) and in quantification of MA and/or MDMA (Bugamelli et al ., 2006; Chafer‐Pericas et al ., 2004; Kaddoumi et al ., 2004; Nakamura et al ., 2006; Wada et al ., 2005). When MS is not an available detection technique, FD can provide selectivity over UV but does not always provide a sensitivity advantage (see Tables 2 and 4).…”

Quantitative Analysis of Drugs in Biological Matrices by HPLC Hyphenated to Fluorescence Detection

“…The LLOQ in this assay represents a 75-fold increase in sensitivity over UV-assays previously reported by these authors. In 2006, Bugamelli et al [42] reported the quantification of a drug of abuse: amphetamine in human urine. The popularity of amphetamine, and its analogues such as ecstasy, can be attributed to their psychotropic effects.…”

Magnetic solid‐phase extraction using magnetic hypercrosslinked polymer for rapid determination of illegal drugs in urine

“…The escalation of the abuse of these drugs has caused serious health and social problems [23]. In response to a growing demand for reliable evidence of AMPs and/or KET use, qualitative and quantitative detection of AMPs and/or KET in biological matrices has been developed using a variety of techniques such as gas chromatography (GC), gas chromatography-mass spectrometry (GC-MS), high-performance liquid chromatography (HPLC), and liquid chromatography-mass spectrometry (LC-MS) [23][24][25][26][27][28][29][30][31]. To meet the growing demands of separation ability and reductions in organic solvent consumption, capillary electrophoresis (CE) has recently become more and more popular and has been extensively applied in the analysis of illegal drugs in court and clinical diagnosis [32,33].…”