摘要
目的:建立高效液相色谱法和电位滴定法测定创新药物 CD-01盐酸盐的含量。方法:高效液相色谱法:色谱柱为 Dia-monsil C_(18)(5μm,4.6mm×250mm);流动相为甲醇-0.01mol·L^(-1)磷酸二氢钾(pH=7.0)(72∶28),流速1.0mL·min^(-1);UV 检测波长为254nm;柱温40℃。电位滴定法以冰醋酸和醋酐为溶剂。所有操作均避光进行。结果:高效液相色谱法:CD-01盐酸盐在2.99-29.9μg·mL^(-1)范围内线性关系良好,r=0.9998;方法精密度 RSD 为0.61%(n=5);平均回收率为100.0%(n=9);检测限0.8ng。电位滴定法:方法精密度 RSD 为0.15%(n=5);平均回收率为99.99%,RSD 为0.09%(n=5)。结论:高效液相色谱法与电位滴定法的测定结果在统计学上无显著性差异。电位滴定法适用性广,测定结果精密,准确度高;高效液相色谱法专属性强,耗样量小。
Objective:To develop an HPLC and a potentiometry titration method for determining CD-01 hydro- chloride,a new chemical entity.Methods:A reversed-phase HPLC was used.The separation was performed on a Diamonsil C_(18) column(4.6mm×250 mm,5μm).The mobile phase was methanol-0.01 mol·L^(-1)KH_2PO_4 (pH=7.0)(72:28)with flow rate of 1.0 mL·min^(-1).The detection was set at 254 nm and the column tempera- ture at 40℃.Acetic acid and acetic anhydride were used as solvent for potentiometry titration.The handling of CD -01 hydrochloride solution was performed in lightproof container under dim light.Results:HPLC:The linear range for CD-01 hydrochloride was 2.99-29.9μg·mL^(-1)(r=0.9998),the precision RSD was 0.61%(n=5),the average recovery was 100.0%(n=9).Potentiometry titration:the precision RSD was 0.15%(n=5),the average recovery was 99.99% with an RSD of 0.09%(n=5).Conclusions:The HPLC method and potentiometry titration method are identical statistically.Potentiometry titration method is accurate and used widely.The HPLC method is sensitive,specific and needs small amount of sample.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2005年第5期530-533,共4页
Chinese Journal of Pharmaceutical Analysis