Direct Screening of Urine for MDMA and MDA by Liquid Chromatography-Tandem Mass Spectrometry*

Abstract

There is a limit in the number of substances detected by commercially available reagents. It is therefore important to have other, complementary techniques. Liquid chromatography-tandem mass spectrometry (LC-MS-MS) may offer one possibility. An LC-MS-MS procedure based on the detection of positive ions after atmospheric pressure chemical ionization (APCI) was developed for direct measurement of 3,4-methylenedioxymethamphetamine (MDMA) and 3,4-methylenedioxyamphetamine in urine. It was compared with Online Amphetamines. The LC-MS-MS methodology showed improved sensitivity (1 00-ng/mL cutoff and specificity with a coefficient of variation of 10%. It was compared to the immunochemical analysis using 1000 clinical patient urine samples. The positive samples were confirmed by gas chromatography-mass spectrometry. The LC-MS-MS method detected almost four times as many samples positive for MDMA compared to the immunochemical method, with no false positives and one false negative. Our study suggests that LC-MS-MS offers an alternative to immunochemical methods in drug of abuse screening.

Fast LC–MS/MS method for the determination of amphetamine, methamphetamine, MDA, MDMA, MDEA, MBDB and PMA in urine

“…The ESCI TM Multi-Mode Ionization Source used enabled switching between ESI and APCI, supplying voltage to the ESI capillary or current to the APCI corona needle without changing the probe. The literature [24][25][26] reports that APCI has been used successfully, but in same cases a derivatization step was used [24]. Other ionization techniques applied were sonic spray ionization [27] and surface-activated chemical ionization [28].…”

“…LC-MS is an interesting alternative, offering highest sample throughput and less sample manipulation. In the literature, several LC-MS methods for the determination of amphetamine and some of its analogues (MA, MDA, MDMA, MDEA or PMA) in urine were found [21][22][23][24][25][26][27][28]. For plasma different LC-MS methods for the determination of amphetamines and designer drugs have been published [24,27,[29][30][31][32].…”

Sensitive Gas Chromatography-Mass Spectrometry Method for Simultaneous Measurement of MDEA, MDMA, and Metabolites HMA, MDA, and HMMA in Human Urine

“…Liquid-liquid (10,15,16 ) and solid-phase extraction (SPE) procedures have been published (17)(18)(19). Capillary electrophoresis-MS (20,21 ) and liquid chromatography-MS (22)(23)(24)(25) assays also are available. In general, methods have included a limited number of compounds and a limited linear range.…”

Theoretical calculations applied to the study of the energetics of reactions of methamphetamine synthesis and to the characterization of reactants, products and by-products

“…Since the solvation energy difference between Table 2 Energies of compounds 6,7,8,9,10 and 11. Compound Energy ( product and reactant is of À2 Kcal/mol, this reaction does not occur with a change in energy.…”

“…[5], liquid chromatography with fluorescence detection [6], liquid chromatography with mass spectrometry (LC-MS) [7], and immunoassay [8]. Recently, MDMA has also been identified in the urine of users via NMR spectroscopy [9].…”