Determination of paramethoxyamphetamine and other amphetamine‐related designer drugs by liquid chromatography/sonic spray ionization mass spectrometry

Abstract

Paramethoxyamphetamine (PMA) is an amphetamine-like designer drug that has emerged recently on the European illicit drug market. This drug has a wicked reputation, as a number of lethal intoxications have occurred. A method using high-performance liquid chromatography coupled to ion trap based mass spectrometry (LC/MS) is described for the determination of this compound together with 3,4-methylenedioxymethamphetamine (XTC or MDMA), amphetamine and 3,4-methylenedioxyamphetamine (MDA) in human matrices. A liquid/liquid extraction (LLE) was applied to whole blood, urine and postmortem tissues. Reversed-phase liquid chromatography was performed on a narrow-bore phenyl-type column at a flow rate of 0.3 mL/min. A switch box allowed disposal of early-eluting irrelevant material to waste, protecting the mass spectrometer from contamination. The column effluent was directed into an ion trap mass spectrometer by a sonic spray ionization (SSI) interface. The method was validated for all three matrices, proving the applicability of SSI even when dealing with complex biological matrices. The within-and between-day precisions were less than 17.5% and accuracy was below 16.2%. Weighted (1/x) quadratic calibration curves were generated ranging from 10 to 1000 ng/mL (blood and urine) or 20 to 2000 ng/g (tissue) and correlation coefficients (r(2)) always exceeded 0.995. In addition, the mass spectrum of PMA is given together with a proposed fragmentation pattern for the obtained LC/MS spectrum. This information can be useful for future identification of PMA with LC/MS in biological matrices as well as in confiscated powders or tablets.

Simple and rapid analysis of four amphetamines in human whole blood and urine using liquid–liquid extraction without evaporation/derivatization and gas chromatography–mass spectrometry

“…Considering that less solvent would produce a more concentrated sample for both whole blood and urine samples, we chose 200 ll of 1-chlorobutane. This volume of extraction solvent was much less than those reported in the literature [10,21,24,25], and was more analyst-and environment-friendly.…”

“…Some researchers have prevented the evaporation of amphetamines by adding acid [9,20], using a low evaporation temperature [18,21], or trapping analytes by means of derivatization before the highly volatile eluate is evaporated to dryness [22]. Even after derivatization, the compounds needed to be evaporated under low temperatures in order to avoid the evaporation of AMP and MAMP [23].…”

High-Performance Liquid Chromatographic Analysis of Drugs of Abuse in Biologic Samples

“…Weighted (1/x) quadratic calibration curves were generated ranging from 10 to 1000 ng/ml (blood and urine) or 20 to 2000 ng/g (tissue) with correlation coefficients > 0.995. 22) Selegiline and its three metabolites were sensitively assayed using a LC-APCI-MS/MS method. Lower limits of quantitation were 0.1 ng/ml for selegiline and Ndesmethylselegiline, and 0.2 ng/ml for MP and AP.…”

Comprehensive Forensic Toxicological Analysis of Designer Drugs

“…(41,(91)(92) Additionally, LC-MS is not limited to non-polar or volatile compounds. (39,(93)(94)(95) Ultra-fast methods can be used when applying high-pressure to the chromatographic system, as is the case with UPLC, or ultra-performance liquid chromatography. More importantly, fragmentation patterns can positively identify compounds when MS n is used.…”

“…More importantly, fragmentation patterns can positively identify compounds when MS n is used. (91) Liquid chromatography has been combined with diode array detection (DAD), (91,112) In addition to commonly employed biological matrices like blood, hair, and urine, several other matrices have been introduced to LC-MS techniques, including oral fluid, (45,61,93,113) vitreous humor (post-mortem), (114) and exhaled breath. (44) Depending on desired sample matrix available, varying extraction methods are available for LC-MS sample preparation; unlike GC-MS, derivatization of analytes is generally not required.…”