寡核苷酸类药物磷的定性定量分析  

Study on phosphorus qualitative and quantitative analysis in oligonucleotide bulk pharmaceuticals

作　　者：李保山 仲婕 朱德领 施明珠 

机构地区：[1]杭州天龙药业有限公司,浙江杭州310021 [2]军科天龙药物研究院,浙江杭州310021

出　　处：《中国医药科学》2013年第8期63-64,108,共3页China Medicine And Pharmacy

基　　金："十二五"国家重大新药创制科技重大专项(2011ZX09102-001-07);"十二五"国家重大新药创制科技重大专项(2011ZX09102-009-09)

摘　　要：目的用钼酸铵比色紫外分光光度法测定抗肝癌药物磷含量。方法用硝酸-高氯酸消解,钼酸铵比色紫外分光光度法测定药品中磷含量。用核磁共振31P-NMR谱,又进一步确定了本品寡核苷酸类化合物磷酸骨架上化学位移为55ppm的PS键。结果分光光度法磷含量测定标准曲线为Y=0.13X+0.0227,r=0.9995,方法的精密度分别为:0.74%,重现性5.6%,回收率99.65%。结论钼酸铵比色紫外分光光度法测定寡核苷酸类抗肝癌药物和抗病毒药物中磷的含量,可操作性强,回收率较高,可为其他核酸类药物测定提供借鉴。31P-NMR谱进一步分析了P在硫代寡核苷酸药物中磷的存在形式。Objective By using ammonium molybdate colorimetric UV spectrophotometric to determine the phosphorus content of the oligonucleotide bulk pharmaceuticals. Methods Digestion with nitric acid -perchloric acid,phosphorus assay was performed by ammonium molybdate colorimetric UV spectrophotometric. Explore the P = S combination test in oligonucleotide by nuclear magnetic resonance spectrum 31p-NMR. Results The standard curve of phosphorus content determination is Y=0.13X＋0.0227, r=0.9995,the precision of the method were 0.74%,reproducibility of 5.6%,the recovery is 99.65%. Conclusion The method established in this article was easy,feasible and had a high recovery,and can be used for reference in other nucleic acid analyses. On the other side,nuclear magnetic resonance spectrum 3Ip-NMR define the peculiar kinds of combination between phosphorus and sulphur in oligonucleotide.

关 键 词：钼酸铵紫外分光光度法 寡核苷酸 磷 

分 类 号：O657.63[理学—分析化学]