Simultaneous identification of amphetamine and its derivatives in urine using HPLC-UV

Abstract

An HPLC-UV method for the simultaneous identification of amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine (MDA) and 3,4-methylenedioxymethamphetamine (MDMA) in urine is described. It includes a rapid extraction procedure of the 4 analogs from urine using Extrelut 3 columns, derivatization with sodium 1,2-naphthoquinone-4-sulphonate (NQS) to obtain highly chromophoric UV-VIS derivatives, and a final HPLC analysis using an ion-pair reversed-phase technique with eluent monitoring at 480 nm. Structural characterization of the derivatives obtained by mass spectrometry is reported. Recoveries of the amphetamines were in the range 80-85% at concentrations of 300 ng/ml. Practical detection limits were 40-60 ng/ml (S/N ratio = 10) for all derivatives. The chromatographic peaks of the NQS derivatized amphetamines are fairly narrow and well resolved. The method is simple, rapid, quite sensitive, and specific for convenient confirmation of preliminary positive results obtained with immunoassays.

Determination of amphetamine-derived designer drugs in human urine by SPE extraction and capillary electrophoresis with mass spectrometry detection

“…The CE-MS analysis allow the quantitative determination of amphetamine derivates comparable in sensitivity, accuracy and precision to LC-MS techniques [14,16].…”

“…To date, the determination of amphetamines in urine samples has been mainly on GC-MS [8][9][10][11][12] and HPLC-DAD [7,[13][14]. In the last few years, the liquid chromatography coupled mass spectrometry (LC-MS) has developed rapidly in forensic and clinical applications as well as in analysis of amphetamines in biological samples [15][16][17].…”

High‐Performance Liquid Chromatographic Analysis of Psychotropic and Endogenous Compounds

“…The methods generally used water/acetonitrile mobile phases operated in gradient mode. All studies reported extraction recoveries of 85-102% for all the analytes, with LLOQs ranging from 5 to 60 ng/ml (Tedeschi et al, 1993;Falco et al, 1996;Hernandez et al, 1997;Al-Dirbashi et al, 1997;Al-Dirbashi et al, 2000;Soares et al, 2001).…”

Identification of beverages and beverage stains by GC/MS using aroma components as indicators

“…Solid-phase extraction is useful for selective extraction of target compounds from various matrices, such as biological samples or food, and has become more popular for the analysis of abused drugs [7,8]. Shimoda et al [9] successfully used a porous polymer beads column to concentrate aroma components in foods.…”