高效液相色谱法对新型吡啶类活性物质XY-4的纯度测定

Determination of purity of new pyridine active substance XY-4 by using high performance liquid chromatography

目的建立新型吡唑[3,4-b]吡啶类活性物质XY-4的高效液相色谱法测定含量的方法。方法采用高效液相色谱法,以Phenomenex Gemini 5μm C18 110(4.6 mm×250 mm,5μm)为色谱柱,甲醇-水(75∶25)为流动相,流速1 ml/min,柱温30℃;检测波长为230 nm。结果 XY-4的量在20~100μg/ml的浓度范围内与峰面积积分值线性关系良好(r=0.9999),平均加样回收率为97.6%,RSD为1.45%。结论该方法简便易行,准确可靠,可用于指导XY-4的合成。

Objective To establish a new method for determination of pyrazole[3,4-b]pyridine active substance XY-4 by using HPLC.Methods The determination was performed on a Phenomenex Gemini 5μm C18 110(4.6 mm×250 mm,5μm)with PDA detector at 230 nm.Methanol(water(75∶25)was used as the mobile phase.The flow rate was 1 ml/min and the column temperature was 30℃.Results The amount of XY-4 had linear relation with peak area when the sample volume was ranged from 20 to 100μg/ml(r=0.9999).The average rate and standard deviation of XY-4 were 97.6%and 1.45%(n=6),respectively.Conclusion The method is simple,accurate and reliable.It can be used to guide the synthesis of XY-4.