摘要
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.
出处
《中国新药杂志》
CAS
CSCD
北大核心
2016年第19期2268-2271,共4页
Chinese Journal of New Drugs
基金
国家自然科学基金资助项目(81170492)
江苏省高校自然科学研究面上项目(10KJB350002)
关键词
盐酸美金刚
柱前衍生
高效液相色谱法
苯甲酰氯
三乙胺
乙腈
memantine hydrochloride
pre-column derivatization
HPLC
benzoyl chloride
triethylamine
acetonitrile