Quantification of MDMA and MDA in abusers' hair samples by semi‐micro column HPLC with fluorescence detection
Biomedical Chromatography – June 01, 2006
Source: OpenAlex
Summary
A highly sensitive method for detecting MDMA and related substances in human hair achieved detection limits as low as 0.15 ng/mg for MDA. Utilizing a semi-micro column high-performance liquid chromatography with fluorescence detection, the technique employed a novel labeling reagent, DIB-Cl, alongside a mobile phase of acetonitrile, methanol, and water. With an impressive precision range of 1.5–6.8% for intra-day assays (n=5) and 2.7–4.7% for inter-day assays (n=5), this method is poised for forensic applications in drug analysis.
Abstract
Abstract A sensitive semi‐micro column high‐performance liquid chromatography with fluorescence detection method was developed for the determination of 3,4‐methylenedioxymethamphetamine (MDMA), 3,4‐methylenedioxyamphetamine (MDA), methamphetamine (MP) and amphetamine (AP) in human hair. 4‐(4,5‐Diphenyl‐1 H ‐imidazol‐2‐yl)benzoyl chloride (DIB‐Cl) and 1‐methyl‐3‐phenylpropylamine were used as labeling reagent and internal standard, respectively. These drugs were extracted from hair into 5% trifluoroacetic acid in methanol, and fluorescent labeled with DIB‐Cl. The separation of DIB‐derivatives was achieved on a reversed‐phase semi‐micro ODS column with an acetonitrile–methanol–water (30:40:30, v/v/v%) mixture as a mobile phase. The limits of detection at a signal‐to‐noise ratio of 3 for MDMA, MDA, MP and AP were 0.25, 0.15, 0.25 and 0.19 ng/mg, respectively. Precision of intra‐ and inter‐day assay as the relative standard deviation were in the range 1.5–6.8% ( n = 5) and 2.7–4.7% ( n = 5), respectively. The proposed method was highly sensitive and able to detect MDMA and its related compounds in small amounts of hair sample, and could be applied to quantification of six abusers' hair samples. Copyright © 2006 John Wiley & Sons, Ltd.