利用31PNMR谱快速测定药物中ATPADPAMP以及磷酸盐的含量.PDF

31 利用 P NMR 谱快速测定药物中ATP、ADP、AMP 以及磷酸盐的含量 * 李添宝 ，罗敬，尹帮少 （湖南师范大学 化学化工学院，湖南 长沙 4 10081） 31 摘要：利用 P NMR 谱对同一样品中ATP、ADP、AMP 以及磷酸钠和焦磷酸钠等含磷物质进行定性 定量分析，得到ATP、ADP 、AMP 在0.004 mol L-1～0.080 mol L-1 ，NaH PO 、Na P O 在0.005 mol L-1～ 2 4 4 2 7 0.100 mol L-1 范围内具有很好的线性关系。该方法精密度为0.40%～1.30%，添加回收率为96.9%～105.2% 。 把该方法应用于ATP 注射液的测定，测得ATP 注射液中的杂质为ADP 和磷酸盐，ATP 的含量符合药典要 求。实验结果表明该方法重现性好、准确度高，而且无需前处理、操作简单、快速、无其他元素的干扰， 是一种全新、可靠的分析ATP、ADP、AMP 以及磷酸盐的方法。 31 关键词： P NMR ；ATP ；ADP ；AMP ；磷酸钠；焦磷酸钠 中图分类号：R917 Rapid determination of ATP、ADP、AMP and phosphate in drug by 31 P NMR spectroscopy * LI Tian–bao ，LUO Jing，YIN Bang-shao (College of Chemistry and Chemical Engineering, Hunan Normal University, Changsha 410081, China) Abstract: The content of ATP, ADP, AMP, sodium phosphate and sodium pyrophosphate were determined by 31P NMR, the linear range of ATP, ADP, AMP were found to be 0.004 mol L-1～0.080 mol L-1, sodium phosphate and sodium pyrophosphate were 0.005mol L-1～0.100 mol L-1.The RSD were 0.40%～1.30%, the recovery were 96.9%～105.2%. The method has been applied to the determination of ATP inj ection, the impurities of ATP inj ection were ADP and sodium phosphate, the content of ATP in line with the requirement of the pharmacopoeia. The results indicated that the method was of good reproducibility, high accuracy, rapid and simple operation ,without pretreatment and interference of other elements, 31P NMR is a new and reliable method of analyzing ATP, ADP, AMP and phosphate. Key words: 31P NMR; ATP; ADP;