Tomita Mamoru, Nakashima Mihoko N, Wada Mitsuhiro, Nakashima Kenichiro
Department of Clinical Pharmacy, Course of Pharmaceutical Sciences, Graduate School of Biomedical Sciences, Nagasaki University, 1-14 Bunkyo-machi, Nagasaki 852-8521, Japan.
Biomed Chromatogr. 2006 Dec;20(12):1380-5. doi: 10.1002/bmc.716.
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 microL) 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 Na(2)HPO(4) aqueous buffer (pH 4.0)-CH(3)CN-CH(3)OH (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 (C(max)), 20 +/- 5 and 100 +/- 10 min (T(max)), respectively.
建立了一种灵敏的高效液相色谱荧光检测法，用于测定人及大鼠全血或血浆样品中的3,4-亚甲基二氧基甲基苯丙胺（摇头丸）和3,4-亚甲基二氧基苯丙胺（MDA）。该方法以4-(4,5-二苯基-1H-咪唑-2-基)苯甲酰氯（DIB-Cl）作为标记物。取少量血样（约100 μL）中的摇头丸和MDA，用乙酸乙酯液液萃取，并在温和条件下（室温10分钟）用DIB-Cl进行衍生化。使用市售的ODS柱，以10 mM柠檬酸-20 mM Na₂HPO₄ 水溶液缓冲液（pH 4.0）-CH₃CN-CH₃OH（50:45:5，v/v/v%）作为等度洗脱剂，可在45分钟内实现DIB-衍生物的良好分离。以1-甲基-3-苯基丙胺（MPPA）作为内标物绘制的校准曲线具有良好的线性（r = 0.999），在信噪比为3时，检测限为0.36 - 0.83 ng/mL。单次腹腔注射摇头丸（2.2 mg/kg）后，可对大鼠全血中的摇头丸和MDA进行6小时的监测。通过三次重复测量获得的摇头丸和MDA的药代动力学参数分别为426 ± 23和39 ± 6 ng/mL（Cmax），20 ± 5和100 ± 10分钟（Tmax）。
