固定相优化液相色谱法对候选新药雷公藤衍生物进行有关物质检查

Application of Phase Optimized Liquid Chromatography for Related Substances Detection in New Drug Candidate of Tripterygiumforrestii Derivative

采用固定相优化液相色谱法(POPLC)建立了候选新药雷公藤衍生物(T8)中有关物质的检查方法。分别采用5种不同类型的固定相色谱短柱对含有T8和有关物质的混合溶液进行实验,流动相为乙腈-水(35∶65,V/V),流速为0.5mL/min,柱温为30℃,检测波长为219nm,获得相应各柱死时间、各组分保留时间和理论板数。经专门软件进行计算拟合,得到优化的色谱柱组合为20mm氰基柱+80mm氨基键合柱。结果表明,在上述优化色谱条件下,10min内可实现T8与有关物质之间的良好分离,并可用于考察T8的强制性破坏溶液。

Phase optimized liquid chromatography（POPLC） was applied for the related substance detection in new drug candidate of T8,one of tripterygiumforrestii derivative.Five column segments with different kind of stationary phases were individually employed to perform basic measurements for mixture solutions of T8 and its related substances.The mobile phase was composed of acetonitrile and water（35 ∶ 65,V/V） with the flow rate of 0.5 mL/min.The column temperature was set at 30 ℃ and the detection was performed at 219 nm.The dead time of the segment columns was determined using a 0.05%（m/V） solution of uracil.The retention times and the theoretical plate numbers of T8 and its six known related substances were obtained from the basic measurements.An optimal stationary phase composition of 100 mm total length with 20 mm cyanopropyl silica（CN column） coupled to 80 mm embedded polar octadecyl silica（EPS column） was calculated by the optimizer sofrware.Good separation was obtained in 10 min for the related substance detection in T8 and its forced degraded solutions,as well.