一种苯并咪唑酮类GSK-3抑制剂的纯度研究

Study on purity of GSK-3 inhibitor benzimidazolone

目的:建立苯并咪唑酮类新型GSK-3抑制剂的纯度测定方法。方法:采用高效液相色谱法,采用Phenomenex Gemini C_(18)110A色谱柱(4.6 mm×250 mm,5μm),甲醇-水(75∶25)为流动相,流速1 m L﹒min^(-1),柱温为30℃,检测波长254 nm。结果:苯并咪唑酮类GSK-3抑制剂(化合物5b)的含量在20~100μg﹒mL^(-1)的浓度范围内与峰面积具有良好的线性关系(r=0.9999),平均加样回收率为100.44%,RSD为0.78%。结论:该纯度测定方法简便高效、实用可靠,可用于指导苯并咪唑酮类新型GSK-3抑制剂的合成及系列衍生物的纯度测定。

Objective: To establish a new method for the purity determination of benzimidazolone derivatives of GSK-3 inhibitor. Method: The determination was performed on a Phenomenex Gemini C18 110 A column(4.6 mm × 250 mm, 5 μm) with PDA detector at 254 nm with methanol-water(75∶25) as the mobile phase. The flow rate was 1 mL﹒min^-1 and the column temperature was 30℃. Result: The content of GSK-3 inhibitor(compound 5 b) showed a good linear relationship with the peak area in the concentration range of 20100 μg﹒mL^-1(r=0.9999). The average recovery rate and the relative standard deviation of compound 5 b were 100.44% and 0.78%, respectively. Conclusion: The method is simple and efficient,practical and reliable, which can be used to guide the synthesis of benzimidazolones, a novel GSK-3 inhibitor, and the purity determination of series of derivatives.