HPLC法和电位滴定法测定创新药物CD-01盐酸盐的含量

Determination of CD-01 Hydrochloride by HPLC and Potentiometry Titration

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.