多波长反相高效液相色谱法对止痛方中几种有效成分含量测定

Analysis Several Active Ingredients of Zhitong Prescription One-time by RP-HPLC Determination

摘要:

目的: 利用多波长反相高效液相色谱法(RP-HPLC)建立对民间验方仲氏止痛散加减后的止痛方中6种有效成分的含量进行同时测定的方法。 方法: 使用Diamond C₁₈色谱柱(4.6 mm×250 mm,5 μm),柱温30℃,甲醇-乙腈-0.1%氨水为流动相,以1 mL·min^-1梯度洗脱,检测波长230 nm(芍药苷)、235 nm(乌头碱、次乌头碱)、280 nm(延胡索乙素)、280 nm(原阿片碱)、235 nm(新乌头碱)。 结果: 6个成分峰面积与浓度呈良好的线性(r>0.999 4),芍药苷、延胡索乙素、原阿片碱、乌头碱、次乌头碱、新乌头碱的加样回收率分别为97.2%(RSD 1.4%),96.5%(RSD 1.2%),102.5%(RSD 0.7%),96.8%(RSD 0.7%),100.8%(RSD 1.1%),98.5%(RSD 1.1%)。 结论: 利用RP-HPLC同时测定止痛方中的几种有效成分,简便易行,为止痛方相关制剂的质量控制提供一定的依据。

Abstract:

Objective: Using reversed-phase high performance liquid chromatography (RP-HPLC) method to analyze 6 ingredients of Zhitong prescription one-time. Method: Using Diamond C₁₈ column (4.6 mm×250 mm, 5 μm), the column temperature was 30℃; methanol acetonitrile 0.1% ammonia water as the mobile phase, 1 mL·min^-1 gradient elution; detection wavelength was 230 nm (paeoniflorin), 235 nm (the aconitine hypaconitine), 280 nm (tetrahydropalmatine), 280 nm (protopine) and 235 nm (mesaconitine). Result: The peak area and concentration of the six components showed good linearity (r>0.999 4) the paeoniflorin aconitine hypaconitine, tetrahydropalmatine protopine, new aconitine the recoveries were 97.2% (RSD 1.4%), 96.5% (RSD 1.2%), 102.5% (RSD 0.7%), 96.8%(RSD 0.7%), 100.8%(RSD 1.1%), 98.5%(RSD 1.1%). Conclusion: By using RP-HPLC simultaneous determination of the active ingredients of the the analgesic prescription of several simple, we can provide a basis for the quality control of the preparation of Zhitong prescription.