Abstract

A GC/MS method for the simultaneous analyses of different amphetamines and ephedrines in urine employing analytical-grade acetic anhydride/pyridine as derivatizing reagents was developed and validated. Solid-phase extraction was performed on the samples, which were then derivatizated and analyzed by GC/MS. The method showed a broad linear dynamic range (25-1000 ng mL-1 with R² > 0.99), high sensitivity (LODs of 0.0140 to 15.33 ng mL-1 and LOQs of 0.0466 to 51.10 ng mL-1), good precision (CV < 6% for intra- and inter-assays), and excellent extraction recovery (87 to 96%) for all the compounds studied. After validation, the method was applied in the analyses of real samples of human urine which were previously determined to contain at least one of such drugs. In all the samples, the amphetamines and ephedrines were promptly quantified, showing that the association of acetic anhydride and pyridine can be conveniently employed as a derivatizing agent.

Highlights

  • Amphetamines and ephedrines constitute the major class of stimulants of the Central Nervous System (CNS)

  • These are the most characteristic ions that show a significant intensity in the full scan mass spectra (Figure 2) of the derivatizated analytes.[16]

  • The unique retention times (Table 1) obtained for each acetylated compound indicates that the derivatization method yielded only one derivative

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Summary

Introduction

Amphetamines and ephedrines constitute the major class of stimulants of the Central Nervous System (CNS). They may cause a decrease in physical and mental fatigue with the consequent increase of alertness, competitiveness, and aggressiveness.[1] These stimulants, especially the synthetic derivatives, have been usually found in rave parties, and illegally abused by weight-room’s users in order to get. A number of reports on the analysis of amphetamines and ephedrines in biological samples using gas or liquid chromatography coupled to mass spectrometry (GC/MS or LC/MS) has been described.[4,5,6] these methods provide satisfactory results, most of them are not general. Vol 20, No 2, 2009 describing the analysis of specific drugs.[7,8,9] On the other hand, only few methods dealing with the detection of ephedrines have been reported.[10,11] As amphetamines have a relatively high polarity and ephedrines are thermically unstable,[12] a derivatization step is usually required

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