3-正丁基苯酞含量及有关物质测定的方法学研究

目的采用反相高效液相色谱法测定 3 正丁基苯酞脂质体的含量及有关物质检查。方法脂质体以 1 0mL 1 0 % (φ)的TritonX— 1 0 0溶解 ,采用ODS色谱柱 ,以0 0 5mol·L-1醋酸钠 乙腈(V∶V =40∶60 )用醋酸调 pH 4 5为流动相 ,流速 1 0mL·min-1,检测波长 2 2 8nm ,柱温 40℃。结果RP HPLC法测定的线性范围为 5 1 6～ 2 5 7 89mmol·L-1,相关系数r=0 9999;脂质体中 3 正丁基苯酞的平均回收率为 99 9% ,RSD =0 46% ,n =9;最低检测限 0 0 98ng;重现性 (RSD =0 68% )良好。结论该法操作简便、快速、准确、专属性强 ,适用于 3 正丁基苯酞的含量测定及其有关物质检查。

Determination of the content and the related substances of 3-n-butylphthalide in liposomes by RP-HPLC

Objective To determine the content and the related substances of 3- n -butylphthalide in liposomes.Method The RP-HPLC method was used.The mobile phase consisted of 0.05 mol·L -1 sodium acetate buffer (pH 4.5)-acetonitrile ( V∶V =4∶6),at a flow-rate 1.0 mL·min -1 and the column temperature 40℃.The detection wavelength was 228 nm.The liposomes were dissolved with 1.0 mL of Triton X-100 ( φ =10%).Results The linear calibration curves were obtained over the range of 5.16～ 257.89 mmol·L -1 ( r =0.999 9 ).The average recovery of 3- n -butylphthalide was 99.86% (RSD=0.46%) in liposomes.The detection limit was 0.098 ng .The precision of the method (RSD=0.68%) was good.Conclusion The method is proved to be suitable for detecting the content and the related substances of 3- n -butylphthalide in liposomes,which offers the advantages of specifity,speed,and sensitivity.