Details

Autor(en) / Beteiligte

• Tomita, Mamoru
• Nakashima, Mihoko N.
• Wada, Mitsuhiro
• Nakashima, Kenichiro

Titel

A simple and sensitive HPLC-fluorescence method for quantification of MDMA and MDA in blood with 4-(4,5-diphenyl-1H-imidazol-2-yl)benzoyl chloride (DIB-Cl) as a label

Ist Teil von

• Biomedical chromatography, 2006-12, Vol.20 (12), p.1380-1385

Ort / Verlag

Chichester, UK: John Wiley & Sons, Ltd

Erscheinungsjahr

2006

Link zum Volltext

Quelle

Wiley Online Library Journals Frontfile Complete

Beschreibungen/Notizen

• A sensitive high‐performance liquid chromatographic method with fluorescence detection to determine 3,4‐methylenedioxymethamphethamine (MDMA) and 3,4‐methylenedioxyamphethamine (MDA) in human and rat whole blood or plasma samples was developed by using 4‐(4,5‐diphenyl‐1H‐imidazol‐2‐yl)benzoyl chloride (DIB‐Cl) as a label. MDMA and MDA in a small amount of blood sample (ca 100 µL) were extracted by liquid–liquid extraction with ethyl acetate, and were derivatized with DIB‐Cl under mild conditions (10 min at room temperature). A good separation of DIB‐derivatives could be achieved within 45 min using a commercially available ODS column with an isocratic eluent of 10 mm citric acid–20 mm Na2HPO4 aqueous buffer (pH 4.0)–CH3CN–CH3OH (50:45:5, v/v/v %). The calibration curves prepared with 1‐methyl‐3‐phenylpropylamine (MPPA) as an internal standard showed good linearity (r = 0.999) with 0.36–0.83 ng/mL detection limit at a signal‐to‐noise ratio of 3. MDMA and MDA in rat whole blood could be monitored for 6 h after a single administration of MDMA (2.2 mg/kg, i.p.). The pharmacokinetic parameters for MDMA and MDA obtained by triplicate measurements were 426 ± 23 and 39 ± 6 ng/mL (Cmax), 20 ± 5 and 100 ± 10 min (Tmax), respectively. Copyright © 2006 John Wiley & Sons, Ltd.