HPLC测定曲匹布通片的含量与有关物质

Determination of the Content of Trepibutone and Related Compounds by HPLC

关键词:  曲匹布通片  高效液相色谱法  含量测定  有关物质  质量控制

Key words:  Trepibutone tablets  HPLC  determination of content  related substances  quality control

摘要:

目的 建立HPLC测定曲匹布通片的含量和有关物质。方法 采用Thermo C₁₈色谱柱(250 mm×4.6 mm，5 μm)，以0.01 mol·L^-1的醋酸铵溶液(用冰醋酸调节pH值至3.0)-甲醇(40∶60)为流动相；检测波长271 nm，流速1.0 mL·min^-1，柱温35 ℃，进样量10 μL。结果 曲匹布通在0.100 5~1.005 2 mg·mL^-1内线性关系良好，平均回收率为100.5%(RSD=0.5%)。曲匹布通及其有关物质能得到很好分离，定量限为0.000 1 ng，检测限为0.000 03 ng，供试品溶液在8 h内的稳定性良好(RSD=0.6%)。结论 该方法简便、准确、重复性好，适用于曲匹布通片的质量控制。

Abstract:

OBJECTIVE To establish an HPLC method for the determination of the content of trpibutone and related substances. METHODS The HPLC system consisted of Thermo C₁₈ column(250 mm×4.6 mm, 5 μm) was used, methanol-buffer(0.01 mol·L^-1 ammonium acetate, adjusted pH to 3.0 by phosphoric acid) (40∶60) was adopted as mobile phase with UV detection at 271 nm. The flow rate was 1.0 mL^-1, column temperature was 35 ℃, injection volume was 10 μL. RESULTS The linear range was 0.100 5-1.005 2 mg·mL^-1. The mean recovery was 100.5%(RSD=0.5%). Trepibutone and related substances were separated well. The limit of quantification was 0.000 1 ng, the limit of detection was 0.000 03 ng. The sample solution was stable within 8 h(RSD=0, 6%). CONCLUSION This method is simple, sensitive and accurate.