Zarghi Afshin, Shafaati Alireza, Foroutan Seyed Mohsen, Khoddam Arash, Madadian Babak
Department of Pharmaceutical Chemistry, School of Pharmacy, Shahid Beheshti University of Medical Sciences, Tehran, Iran.
Sci Pharm. 2010 Oct-Dec;78(4):847-56. doi: 10.3797/scipharm.1008-17. Epub 2010 Oct 5.
A rapid, sensitive and reproducible HPLC method was developed and validated for the analysis of memantine in human plasma after derivatization with o-phthaldialdehyde (OPA) and fluorescence detection. Amantadine was used as internal standard. The derivatized memantine and amantadine were eluted in less than 10 min with no interference from endogenous plasma peaks. The analysis was carried out on a monolithic silica column (Chromolith Performance RP-18e, 100Ã4.6 mm). The mobile phase was composed of a mixture of acetonitrile and 0.025 M phosphate buffer (50:50, v/v, pH=4.6) with a flow rate of 2.5 mLmin(â1). The excitation and emission wavelengths were set at 335 nm and 440 nm respectively. The assay enables the measurement of memantine for therapeutic drug monitoring with a lower quantification limit of 2 ngmL(â1). The method involves simple extraction procedure and analytical recovery was 82.8Â 0.9%. The calibration curve was linear over the concentration range 2â80 ngmL(â1). The coefficients of variation for inter-day and intra-day assay were found to be less than 8%. The method was successfully applied to pharmacokinetic studies in humans.
建立了一种快速、灵敏且可重复的高效液相色谱法，并进行了验证，用于分析经邻苯二甲醛（OPA）衍生化和荧光检测后人体血浆中的美金刚。金刚烷胺用作内标。衍生化的美金刚和金刚烷胺在不到10分钟内洗脱，无内源性血浆峰干扰。分析在整体硅胶柱（Chromolith Performance RP - 18e，100×4.6 mm）上进行。流动相由乙腈和0.025 M磷酸盐缓冲液（50:50，v/v，pH = 4.6）的混合物组成，流速为2.5 mL·min⁻¹。激发波长和发射波长分别设定为335 nm和440 nm。该测定法可用于治疗药物监测中美金刚的测量，定量下限为2 ng·mL⁻¹。该方法提取步骤简单，分析回收率为82.8±0.9%。校准曲线在2 - 80 ng·mL⁻¹浓度范围内呈线性。日间和日内测定的变异系数均小于8%。该方法成功应用于人体药代动力学研究。
