Michail Karim, Daabees Hoda, Beltagy Youssef, Elkhalek Magdy Abd, Khamis Mona
J AOAC Int. 2013 Nov-Dec;96(6):1302-7. doi: 10.5740/jaoacint.11-080.
A validated HPLC-UV method is presented for the quantification of urinary memantine hydrochloride, a novel medication approved to treat moderate and advanced cases of Alzheimer's disease. The drug and amantadine hydrochloride, the internal standard, were extracted from human urine using SPE. The extract was then buffered and derivatized at room temperature using o-phthalaldehyde in the presence of N-acetyl-L-cyteine. Chromatographic separation of the formed derivatives was achieved on a C18 column using methanol-water mobile phase adjusted to pH 7 and pumped isocratically at 1 mL/min. The UV detector was set at 340 nm. The chromatographic run time did not exceed 10 min. The LOD and LOQ were 8 and 20 ng/mL, respectively. The RSDs for intraday and interday precisions did not exceed 5.5%. The method was used to monitor memantine hydrochloride in human urine in order to determine an appropriate sampling interval for future noninvasive therapeutic drug monitoring. The assay could also be applied to the determination of amantadine. The described assay showed that a postdosing time interval of 25-75 h seems adequate for sampling and monitoring memantine in urine.
本文介绍了一种经过验证的高效液相色谱-紫外检测法，用于定量测定盐酸美金刚，这是一种被批准用于治疗中度和重度阿尔茨海默病的新型药物。使用固相萃取法从人尿中提取药物和内标盐酸金刚烷胺。然后将提取物缓冲，并在室温下于N-乙酰-L-半胱氨酸存在的条件下用邻苯二甲醛进行衍生化。在C18柱上，使用pH值调至7的甲醇-水流动相，以1 mL/min等度洗脱，实现对生成衍生物的色谱分离。紫外检测器设置在340 nm。色谱运行时间不超过10分钟。检测限和定量限分别为8和20 ng/mL。日内和日间精密度的相对标准偏差不超过5.5%。该方法用于监测人尿中的盐酸美金刚，以确定未来无创治疗药物监测的合适采样间隔。该测定法也可用于测定金刚烷胺。所描述的测定法表明，给药后25至75小时的时间间隔似乎足以对尿中美金刚进行采样和监测。
