柱前衍生化HPLC法测定盐酸美金刚的含量

Determination of memantine hydrochloride with pre-column derivatization HPLC

目的：建立一种柱前衍生化HPLC测定盐酸美金刚含量的方法。方法：色谱柱为Sun FireTMC18柱（150 mm×4.6 mm,5μm）,流动相为乙腈-水（80∶20）,流速为1.0 m L·min^-1,检测波长为254 nm;以苯甲酰氯为衍生化试剂,三乙胺为缚酸剂,经衍生化后进样测定。结果：在药物溶液中依次加入5%三乙胺乙腈溶液4 m L,5%苯甲酰氯乙腈溶液2 m L,于40℃水浴中振摇反应10 min,然后用乙腈定容后即可进行测定。结果表明,得到的供试溶液在12 h内稳定;在0.040 00-0.800 0 mg·m L^-1浓度范围内线性良好,线性方程Y=1.403×10^7X＋1.215×10^5,r=0.999 8;6份样品的含量平均值为99.21%,重复性RSD为1.78%（n=6）;测定结果与滴定法相比基本一致。结论：本方法操作简便,结果准确可靠、重现性好,可用于盐酸美金刚含量的测定。

Objective： To establish a pre-column derivatization HPLC method for determination of memantine hydrochloride. Methods： 4 m L 5% triethylamine acetonitrile solution and 2 m L 5% benzoyl acetonitrile solution were added into the drug solution sequentially as deacid and derivatization reagents respectively,and derivatization reaction was conducted through shaking the mixture in water bath（ 40 ℃） for 10 min. Then acetonitrile was added to the fixed volume to obtain the final sample solution for HPLC determination. The separation and determination were achieved on a Sun Fire^TM C18 column（ 150 mm × 4. 6 mm,5 μm） with the mobile phase of acetonitrile-water（ 80∶ 20）. The flow rate was 1. 0 m L·min^-1and the wavelength was set at 254 nm. Results： The sample solution was stable within 12 h and he linear range of the calibration curve was 0. 040 00 - 0. 800 0 mg·m L^-1. The average content of 6 samples was 99. 21%,and the RSD was 1. 78%（ n = 6）. Conclusion： The method is simple,accurate,reliable,and reproducible. The derivatization reaction is rapid with good stability,which can be used for the determination of memantine hydrochloride.