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目的建立滋肾健脾液(生地、枸杞、制首乌等)中梓醇及大黄素含量测定的HPLC方法。方法采用ZORBAX SB-AqAgilent 1100(150 mm×4.6 mm,5μm)色谱柱。梓醇含量测定色谱条件为:以乙腈-水(0.6:99.4,V/V)为流动相,流速1 mL·min~(-1),检测波长210 nm,柱温25℃。大黄素含量测定色谱条件为:以甲醇-0.1%磷酸(80:20,V/V)为流动相,流速1 mL·min~(-1),检测波长290 nm,柱温25℃。结果梓醇质量浓度在0.024 08～0.240 8 g·L~(-1)内与峰面积呈良好的线性关系(r=0.9999,n=6),低、中、高浓度的对照品溶液的加样回收率分别为97.54%、99.46%、101.35%;大黄素质量浓度在0.81～8.10mg·L~(-1)内与峰面积呈良好的线性关系(r=0.999 9,n=6),低、中、高浓度的对照品溶液的加样回收率分别为97.74%、100.18%、100.66%。结论本法简便、准确、专属性强,可用于该制剂中梓醇及大黄素含量测定。
Objective To establish a HPLC method for the determination of sterols and emodins in Zishenjianpi liquid (rehabilitate earthworm, aphid, and Shouwu, etc.). The method was performed using a ZORBAX SB-AqAgilent 1100 (150 mm x 4.6 mm, 5 μm) column. The sterol content was determined by chromatographic conditions: acetonitrile-water (0.6:99.4, V/V) as the mobile phase, flow rate of 1 mL·min-1, detection wavelength at 210 nm, and column temperature at 25°C. The emodin content was determined by chromatographic conditions: methanol-0.1% phosphoric acid (80:20, V/V) as mobile phase, flow rate of 1 mL·min-1, detection wavelength at 290 nm, column temperature at 25°C. Results The sterol content in the range of 0.024 08 to 0.240 8 g·L -1 showed a good linear relationship with the peak area (r=0.9999, n=6). The addition of low, medium, and high concentrations of the reference solution showed a good linear relationship. The recovery rates of the samples were 97.54%, 99.46% and 101.35%, respectively; the emodin concentration ranged from 0.81 to 8.10 mg·L -1 and showed a good linear relationship with the peak area (r=0.999 9, n=6). The recoveries of the low, medium, and high concentrations of the reference solutions were 97.74%, 100.18%, and 100.66%, respectively. Conclusion This method is simple, accurate, and highly specific. It can be used for the determination of sterols and emodin in this preparation.