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目的建立RP-HPLC法同时测定护肝剂中马钱素、芍药苷、野黄芩苷、黄芩苷、黄芩素、五味子甲素、五味子乙素、五味子丙素和熊果酸9种中药活性成分,为护肝剂的制剂质量提供保障。方法采用安捷伦Zorbax SB-C18(150 mm×4.6mm,5μm)色谱柱;流动相为乙腈-0.1%磷酸水溶液,梯度洗脱,体积流量1.0 m L/min;紫外检测波长为236、280、210 nm;柱温30℃;进样量为5μL。结果马钱素、芍药苷、野黄芩苷、黄芩苷、黄芩素、五味子甲素、五味子乙素、五味子丙素和熊果酸的最低检测限分别为12.0、2.60、5.75、9.75、14.39、19.06、14.90、15.63、16.08 ng;线性范围分别为583.33~18.229、916.67~28.65、541.67~16.93、416.67~13.02、500.00~15.63、458.33~14.32、625.00~19.53、458.33~14.32、1 000.00~31.25 mg/L;平均加样回收率分别为103.51%、104.19%、95.16%、96.71%、105.61%、96.12%、97.09%、96.87%、105.90%;精密度RSD分别为1.25%、1.31%、1.91%、1.88%、1.95%、1.45%、1.66%、1.52%、1.33%;重复性RSD分别为1.39%、1.41%、1.87%、1.91%、1.79%、1.45%、1.32%、1.71%、1.49%;稳定性RSD分别为1.36%、1.22%、1.87%、1.91%、1.93%、1.56%、1.39%、1.78%、1.61%。6批护肝剂中含马钱素、熊果酸、芍药苷、野黄芩苷、黄芩苷、黄芩素、五味子甲素、乙素及丙素的平均质量浓度分别在216.5~222.5、40.8~42.8、125.4~136.3、144.0~147.3、1 640.8~1 947.3、497.5~515.0、15.0~17.3、33.6~36.0、3.0~3.9 mg/L。结论该方法简便、灵敏度高、重复性好、平均回收率高,是检测护肝剂中马钱素、芍药苷、野黄芩苷、黄芩苷、黄芩素、五味子甲素、五味子乙素、五味子丙素和熊果酸的可信方法。
OBJECTIVE To establish a RP-HPLC method for the simultaneous determination of trace active ingredients of loganin, paeoniflorin, wild baicalin, baicalin, baicalein, schisandrin, schisandrin, schisandrin and ursolic acid in Hugan formula. For the protection of the quality of Hugan preparations. Methods Agilent Zorbax SB-C18 column (150 mm × 4.6 mm, 5 μm) was used. The mobile phase consisted of acetonitrile-0.1% phosphoric acid solution with a gradient elution volume of 1.0 mL / min. The UV detection wavelength was 236, 280, 210 nm; column temperature 30 ℃; injection volume of 5μL. Results The detection limits of loganin, paeoniflorin, wild baicalin, baicalin, baicalein, schisandrin, schisandrin, schisandrin and ursolic acid were 12.0, 2.60, 5.75, 9.75, 14.39, 19.06 , 14.90,15.63,16.08 ng respectively; the linear range was 583.33 ~ 18.229,916.67 ~ 28.65,541.67 ~ 16.93,416.67 ~ 13.02,500.00 ~ 15.63,458.33 ~ 14.32,625.00 ~ 19.53,458.33 ~ 14.32,1000.00 ~ 31.25 mg / L, and the average recoveries were 103.51%, 104.19%, 95.16%, 96.71%, 105.61%, 96.12%, 97.09%, 96.87%, 105.90%, respectively. The precision RSDs were 1.25%, 1.31%, 1.91% 1.81%, 1.95%, 1.45%, 1.66%, 1.52%, 1.33%, respectively; The RSDs of stability were 1.36%, 1.22%, 1.87%, 1.91%, 1.93%, 1.56%, 1.39%, 1.78%, 1.61%, respectively. The average mass concentrations of loganin, ursolic acid, paeoniflorin, paeoniflorin, baicalin, baicalein, schisandrin, acenaphthene and propranolol in six batches of hepatoprotective drugs were 216.5 ~ 222.5 and 40.8 ~ 42.8 , 125.4 ~ 136.3, 144.0 ~ 147.3, 1 640.8 ~ 1 947.3, 497.5 ~ 515.0, 15.0 ~ 17.3, 33.6 ~ 36.0, 3.0 ~ 3.9 mg / L. Conclusion The method is simple, high sensitivity, good reproducibility, high average recovery rate, is the detection of hepatoporphyrin, camellia, wild baicalin, baicalin, baicalein, Schisandrin A, Schisandrin B, Schisandra B Credible and ursolic acid credible method.