CD-01盐酸盐中有关物质的HPLC法检测及稳定性考察

目的用HPLC法检测新药CD 01盐酸盐中有关物质,并进行稳定性考察。方法色谱柱为Diamonsil C18柱(4.6 mm×250 mm,5μm),流动相为甲醇0.01 mol.L-1KH2PO4(pH=6.0,体积比为2∶1),UV检测波长为220 nm,柱温为40℃。所有操作均避光进行。结果CD 01盐酸盐与其中的有关物质、降解产物能够得到良好的分离;CD 01盐酸盐的最低检测量为0.5 ng;在光照条件下,CD 01盐酸盐颜色由类白色变为淡黄色,有关物质含量稍有增加,CD 01盐酸盐含量稍有下降;在其他影响因素试验、加速试验和长期试验中,CD 01盐酸盐的外观性状、有关物质含量及CD 01盐酸盐的含量均无明显变化。表明CD 01盐酸盐在贮存过程中基本稳定,符合新药指导原则中对原料药稳定性的要求。结论HPLC法可作为CD 01盐酸盐原料药稳定性研究的灵敏、可靠的检测方法。

HPLC determination of the related substances of CD-01 hydrochloride and its stability

Objective To develop an HPLC method for determining the related substances and stability of(CD01) hydrochloride,a new drug candidate.Methods The separation was performed on a Diamonsil C_(18)((4.6 mm)× 250 mm,5 μm) column.The mobile phase was methanol-0.01mol·L~(-1)KH_2PO_4(pH=6.0,V∶V=(2∶1))with flow rate of 1.0 mL·min~(-1).The dection was set at 220 nm and the column temperature at 40℃.Results The related substances and degradation products of CD01 hydrochloride can be completely separated from CD01 hydrochloride.The detection limit of CD01 hydrochloride was 0.5 ng.The color of CD01 hydrochloride changed from white to light-yellow under light and related substance increased slightly,while it was found unchanged under other test conditions in the stability study.Conclusions The HPLC method is sensitive and reliable for the stability determination of CD01 hydrochloride.