高效液相色谱法测定前列泰片中山萘素的含量

Determination of Kaempferol in Qianlie Tai Tablet by HPLC

  • 摘要: 建立了测定中药复方制剂前列泰片中山萘素含量的高效液相色谱方法.采用Kromasil C18色谱柱(5 μm,250 mm×4.6 mm),以甲醇∶0.1%磷酸溶液=62∶38(V/V)为流动相,流速1.0 mL/min,检测波长为366 nm.对样品水解过程中各个影响因素进行了考察,获得优化的水解条件为采用4.5 mol/L盐酸溶液,80 ℃水浴上水解1.5 h.山萘素在0.061~ 610 μg/mL范围内峰面积与浓度呈良好的线性关系(r为0.9999),最低检出限为0.03 μg/mL, 平均加标回收率为95.4%,RSD为1.4%.该方法简便、准确、重现性好,可用于前列泰片的质量控制.

     

    Abstract: A high performance liquid chromatographic method was developed for the determination of kaempferol in Qianlie Tai Tablet, a traditional Chinese medicinal preparation. The optimized method was achieved for the separation and detection of kaempferol using Kromasil C18 column (5 μm, 4.6 mm×250 mm) as the stationary phase; a methanol∶0.1% aqueous phosphoric acid solution (62∶38,V/V) as the mobile phase at a flow rate of 1.0 mL/min, 366 nm as the detection wavelength. Sample hydrolyzing procedure was intensively explored, treating of hydrolysis time, temperature and hydrochloric acid concentration. Kaempferol showed good relationship at the range of 0.061~610.000 μg/mL. The correlation coefficient of the calibration curve was 0.9999. The detection limit was 0.03 μg/mL at a signal\|to\|noise ratio of 3. The average recovery of kaempferol was 95.4% with a relative standard derivation (RSD) of 1.4%. The results showed that the method is simple, accurate and repeatable and it is suitable for quality control of Qianlie Tai Tablet.

     

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