基于HPLC波长切换法对芪归通便合剂中六种成分的含量测定

Determination of six components in Qiguitongbian Heji based on HPLC wavelength switching method

目的建立高效液相波长切换法同时测定芪归通便合剂中6种成分的含量。方法采用Diamonsil C18色谱柱(250 mm×4.6 mm,5μm);以甲醇-乙腈(1∶1)与0.1%甲酸溶液为流动相,梯度洗脱;流速0.8 m L/min;柱温30℃。结果松果菊苷、毛蕊花糖苷、毛蕊异黄酮葡萄糖苷、芒柄花素、白术内酯Ⅲ、白术内酯Ⅰ6个成分在12.09~241.80μg/m L(r=0.999 2)、5.51~110.20μg/m L(r=0.999 5)、2.55~51.00μg/m L(r=0.999 8)、3.94~78.80μg/m L(r=0.999 1)、2.08~41.60μg/m L(r=0.999 9)、1.91~38.20μg/m L(r=0.999 4)范围内,与峰面积线性关系良好;平均加样回收率(RSD)分别为99.47%(RSD=1.08%)、98.37%(RSD=1.54%)、96.99%(RSD=1.40%)、98.05%(RSD=0.88%)、98.70%(RSD=1.25%)、97.64%(RSD=0.98%)。结论本文建立的HPLC波长切换法同时测定芪归通便合剂中的6个成分含量,可作为芪归通便合剂全面可靠的质量控制方法。

Objective To develop a high performance liquid chromatography method for determination of six components in Qiguitongbian Heji simultaneously. Methods The Diamonsil C18（ 250 mm × 4. 6 mm,5 μm） chromatographic column was adopted; the mobile phase was methanol-acetonitrile（ 1∶ 1） and 0. 1% formic acid solution with gradient elution,at a flow rate of 0. 8 m L/min,and the column temperature was set at 30 ℃. Results The linear response range of echinacoside,verbascoside,calycosin7-O-β-D-glucopyranoside,formononetin,atracylenolide Ⅲ and atracylenolideⅠ were 12. 09 - 241. 80 μg/m L（ r = 0. 999 2）,5. 51 - 110. 20 μg/m L（ r = 0. 999 5）,2. 55 - 51. 00 μg/m L（ r = 0. 9998）,3. 94 - 78. 80 μg/m L（ r = 0. 999 1）,2. 08 - 41. 60 μg/m L（ r = 0. 999 9）,and 1. 91 - 38. 20 μg/m L（ r = 0. 999 4）,respectively. The average recoveries and the corresponding RSD were 99. 47%（ 1. 08%）,98. 37%（ 1. 54%）,96. 99%（ 1. 40%）,98. 05%（ 0. 88%）,98. 70%（ 1. 25%） and 97. 64%（ 0. 98%）,respectively. Conclusion This HPLC wavelength switching method has been successfully established for simultaneous determination of 6 components in Qiguitongbian Heji. The method is helpful for the quality control of Qiguitongbian Heji.