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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=1.403×107X+1.215×105,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 the determination of memantine hydrochloride. Methods: The column was a Sun FireTMC18 column (150 mm × 4.6 mm, 5 μm) with a mobile phase of acetonitrile-water (80:20) at a flow rate of 1.0 mL · min-1 and a detection wavelength of 254 nm. Derivatization reagent, triethylamine as acid-binding agent, after derivatization injection determination. Results: 4 mL of 5% triethylamine-acetonitrile solution and 2 mL of 5% benzoyl chloride-acetonitrile solution were sequentially added to the drug solution and shaken in a water bath at 40 ° C. for 10 min, then fixed with acetonitrile Determination. The results showed that the obtained solution was stable within 12 h. The linearity was linear over the concentration range of 0.040 00-0.800 mg · mL -1. The linear equation was Y = 1.403 × 107X + 1.215 × 105, r = 0.999 8. The average content of the sample was 99.21% and the repeatability RSD was 1.78% (n = 6). The results of the determination were basically the same as those of the titration method. Conclusion: The method is simple, accurate, reliable and reproducible. It can be used to determine the content of memantine hydrochloride.