Quantification of MDMA and MDA in abusers' hair samples by semi‐micro column HPLC with fluorescence detection
Shinichi Nakamura, Mamoru Tomita, Mitsuhiro Wada, Heesun Chung, Naotaka Kuroda, Kenichiro Nakashima
Biomedical Chromatography June 1, 2006 DOI: 10.1002/bmc.670 via OpenAlex
Summary
AI-generated from the abstractA sensitive method using high-performance liquid chromatography with fluorescence detection was developed to measure MDMA, MDA, methamphetamine, and amphetamine in human hair. Drugs were extracted from hair using trifluoroacetic acid in methanol and labeled with a fluorescent reagent. Separation was achieved on a reversed-phase column. Detection limits for MDMA, MDA, methamphetamine, and amphetamine were 0.25, 0.15, 0.25, and 0.19 ng/mg, respectively. Assay precision ranged from 1.5% to 6.8% for intra-day and 2.7% to 4.7% for inter-day measurements. The method was sensitive enough to detect these compounds in small hair samples and was applied to quantify drugs in six abusers' hair.
Study at a glance
| Characteristics | Method development and validation Peer reviewed |
|---|---|
| Population | Human hair samples from six abusers |
| Topics | MDMA |
| Keywords | Chemistry Trifluoroacetic acid Detection limit High-performance liquid chromatography Reagent |
| Citations | 24 |
| Key finding | The developed method achieved detection limits of 0.15–0.25 ng/mg for MDMA, MDA, methamphetamine, and amphetamine in human hair with good precision. |
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.