冻干鲜地黄生地黄中梓醇和毛蕊花糖苷的含量比较

Comparative Study on Catalpol and Verbascoside Content in Freeze-dried,Fresh and Radix Rehmannia

目的建立HPLC法测定地黄不同炮制品中梓醇和毛蕊花糖苷含量的方法,并对冻干地黄、鲜地黄、生地黄中梓醇和毛蕊花糖苷的含量进行比较测定。方法从产地采集鲜地黄,同时炮制得冻干地黄与生地黄,采用HPLC法直接测定。梓醇色谱条件:Waters XTerra C_(18)柱(250mm×4.6mm,5μm),流动相0.1%磷酸水,流速1.0mL/min,检测波长210nm;毛蕊花糖苷色谱条件Diamonsil C_(18)色谱柱(150mm×4.6mm,5μm),以甲醇(A)-0.1%磷酸水溶液(B)为流动相梯度洗脱,流速为1.0m L/min,检测波长334nm。结果梓醇和毛蕊花糖苷的回归方程分别为Y=16500X-34445(r=0.9993)、Y=31535X-26765(r=0.9996);平均加样回收率分别为95.9%(RSD 0.85%)和95.8%(RSD 0.83%);冻干地黄中梓醇平均含量是生地黄的1.23倍,毛蕊花糖苷平均含量是生地黄的1.17倍。结论该方法操作简便,结果准确、重复性好,可用于地黄不同炮制品的质量评价;冷冻干燥法可减少地黄中梓醇和毛蕊花糖苷的损失。

Objective HPLC was established to determine content of the different processed products of Catalpol and Mullein glucoside,and study on Catalpol and Verbascoside content in freeze-dried Rehmannia root,fresh Rehmannia and Radix Rehmannia,and provide the basis for its quality evaluation. Methods Fresh radix rehmanniae was collected from the place of origin,freeze-dried Radix Rehmanniae and Radix Rehmanniae were prepared simultaneously. The method was directly determined by HPLC. Catalpol chromatographic conditions： Waters XTerra C18 column（ 250 mm × 4. 6 mm,5μm）,with mobile phase consisted of 0. 1% phosphoric acid solution,the flow rate of 1. 0 m L/min,the detective wavelength was set at 210 nm; Mullein glucoside chromatographic conditions Diamonsil-C18 column（ 150 mm × 4. 6 mm,5μm）,with mobile phase consisted of methanol（ A）-0.1% phosphoric acid solution（ B） with gradient elution,the flow rate was 1. 0 m L/min,the detection wavelength was 334 nm. Results The regression equation of catalpol and Mullein glycoside were Y = 16500 X-34445（ r = 0. 9993）,Y = 31535 X-26765（ r= 0. 9996）,respectively; The average recovery rate was 95. 9%（ RSD 0. 85%） and 95. 8%（ RSD 0. 83%）,respectively; freeze-dried Rehmanniae average content of Catalpol is 1. 23 times as much as Radix Rehmanniae,average content of Verbascoside is 1. 17 times. Conclusion This method is simple to operate,the results are accurate and repeatability. It can be used for the quality evaluation of different processed products of Radix Rehmanniae. The freeze drying can reduce the loss of Catalpol and Glucoside in Radix Rehmannia.