Analysis of ecstasy with a monolithic reversed-phase column

Abstract

SummaryA new, rapid, and precise liquid chromatographic method has been developed for simultaneous identification and quantification of amphetamine, N-methyl-3,4-methylenedioxymetamphetamine, N-ethyl-3,4-methylenedioxymetamphetamine, and N-methyl-l-(3,4-methylenedioxyphenyl)-2-butanamine in the presence of other constituents. The compounds were separated on a monolithic column with a gradient prepared from acetonitrile and 20 mM monobasic potassium buffer at a flow rate of 1.5 mL min 1 .Quantitation was performed with metoclopramide as internal standard. Use of different flow rates was investigated and enabled reduction of the separation time from 11 to 3.5 min for seven substances. The method was then applied to ten seized tablets to identify and quantify their active ingredients.als is now available commercially [16]. These Chromolith columns (Merck, Darmstadt, Germany), described as 'monolithic' in nature, consist of one rod of continuous porous silica [17]. Because of their special structure, these columns generate little back-pressure when high mobile-phase flow rates are used and therefore enable faster separations [18 20]. Thus the limitation of high back-pressures capable of destroying a packed column is of minor interest when using monolithic columns. Part of the development of our method was evaluation of this advantage when using the Chromolith SpeedROD RP-18e HPLC column to analyze the amphetamines.

Direct analysis of methcathinone from crude reaction mixture by flowing atmospheric‐pressure afterglow mass spectrometry

“…Fast analysis of such mixtures can be a time-consuming task, as frequently the sample has to be purified before mass spectrometric analysis. There are several methods available for the analysis of illicit drugs: for example, amphetaminetype stimulants (ATS) have been analyzed by thin-layer chromatography (TLC), [3] gas chromatography/flame ionization detection (GC/FID ), [4][5][6] gas chromatography/mass spectrometry (GC/MS), [7,8] high-performance liquid chromatography (HPLC) with diode-array [5,9] or fluorescence detection, [10] and Fourier transform infrared spectroscopy (FTIR), [11] or occasionally by 1 H-NMR, [12] capillary electrophoresis (CE), [13] solid-phase-microextraction-gas chromatography (SPME-GC), [14] and gas chromatography/Fourier transform infrared spectroscopy (GC/FTIR). [15] GC/MS is still the most frequently used approach for analysis of drugs as it provides efficient separation and highly specific spectral data on individual compounds in a complex mixture.…”

Chemiluminescence detection of MDMA in street drug samples using tris(2,2′‐bipyridine)ruthenium(III)

“…Preliminary ‘at‐scene’ identification of the drug class can be performed using colorimetric spot tests (such as the Marquis reagent), but further testing is necessary to indisputably confirm the presence of individual amphetamines within a sample, and to enable quantification. Due to the complex mixtures of compounds that are found within street drug samples, analytical separations, such as gas chromatography (GC) or high performance liquid chromatography (HPLC), are necessary to detect individual components . Therefore, forensic laboratories would benefit from the development of more rapid and selective analysis techniques targeted towards specific illicit substances.…”

Simultaneous HPLC-Determination of Nortriptyline and Fluphenazine in One Minute Using Monolithic Stationary Phase

“…The combination of nortriptyline and fluphenazine is compounds in pharmaceutical dosage forms or biological samples, such as sildenafil, [37] lamivudine, [38] parabenes and triamcinolone in cream formulation, [39] ecstasy, [40] fenfluramine, temazepam, oxazepam, and tamoxifen, [41] mianserin, [42] cephalosporin antibiotics in pharmaceuticals and body fluids, [43] p-amino salicylic acid, [44] corticosteroids in tablets, [45] glimepirid and glibenclamid, [46] acyclovir, [47] rifampicin, [48] tetracyclines, [49] levetiracetam, [50,51] and famotidine and fluoroquinolones. [52] The aim of this study is to establish a fast HPLC-method for simultaneous determination of nortriptyline and fluphenazine depending on the advantage of monolithic stationary phase, which can be used at high flow rates.…”