摘要
目的:建立2,4-二硝基氟苯柱前衍生-高效液相色谱法测定双嘧达莫原料药中的哌啶含量。方法:供试品用甲醇溶解后,经2,4-二硝基氟苯衍生,乙腈定容,采用高效液相色谱仪测定。结果:哌啶含量在0.03981μg/mL~0.1493μg/mL线性关系良好,相关系数r=0.9966,检出限为0.02%。在精密度实验中,其RSD%为3.6%~5.5%。在限度50%、限度100%、限度200%的添加水平下,加标回收率为93.4%~106.0%。结论:该方法专属性良好、灵敏度高、测定结果准确可靠,可用于测定双嘧达莫原料药中的哌啶残留。
Objective: A method for the determination of piperidine in dipyridamole active pharmaceutical ingredients by HPLC with pre-column derivatization of 2,4-dinitrofluorobenzene was established. Methods: The sample was dissolved in methanol, derivated by 2, 4-dinitrofluorobenzene, acetonitrile, and determined by HPLC. Results: There was a good linear relationship between piperidine content at 0.03981 μg/mL ~ 0.1493 μg/mL, the linear correlation coefficient r=0.9966, and the limit of detection was 0.02%. In the precision experiment, the RSD was 3.6% ~ 5.5%. At the addition level of 50%, 100% and 200%, the standard recovery was 93.4% ~ 106.0%. Conclusion: This method has good specificity, high sensitivity, accurate and reliable results, and can be used for the determination of piperidine residues in dipyridamole active pharmaceutical ingredients.
出处
《大众科技》
2021年第7期32-34,7,共4页
Popular Science & Technology
关键词
高效液相色谱法
双嘧达莫原料药
哌啶
high performance liquid chromatography
dipyridamole active pharmaceutical ingredients
piperidine
