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[摘要]
目的 建立同时测定接骨丸中芍药苷、柚皮苷、橙皮苷、丹酚酸B、丹参酮ⅡA的HPLC-DAD方法。方法 采用高效液相色谱波长切换法。Megres C18色谱柱(250 mm×4.6 mm,5 μm);以乙腈-0.1%磷酸溶液为流动相,进行梯度洗脱;检测波长切换为0~15 min为230 nm、15~45 min为280 nm、45~68 min为270 nm;体积流量1.0 mL/min;柱温30 ℃;进样体积10 μL。结果 芍药苷在35.27~352.70 ng、柚皮苷在8.625~86.250 μg、橙皮苷在53.11~531.10 μg、丹酚酸B在19.34~193.40 μg、丹参酮ⅡA在2.142~21.420 μg时进样量与峰面积积分值的线性关系良好。芍药苷、柚皮苷、橙皮苷、丹酚酸B、丹参酮ⅡA的平均回收率分别为100.47%、96.78%、97.45%、100.25%、99.94%,RSD值分别为0.48%、1.07%、1.11%、1.18%、1. 83%。结论 本法简便、快速、准确,可同时测定接骨丸中芍药苷、柚皮苷、橙皮苷、丹酚酸B、丹参酮ⅡA。
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[Abstract]
Objective To establish a quantification method for simultaneous determination of paeoniflorin, naringin, hesperidin, salvianolic acid B, and tanshinone ⅡA in Jiegu Pills by HPLC-DAD. Methods HPLC simultaneously with changing ultraviolet-visible wavelength was used. Megres C18 column (250 mm × 4.6 mm, 5 μm) was used with acetonitrile-0.1% phosphoric acid solution as mobile phase in gradient elution mode. The detection wavelengths were set at 230 nm (retention time 0-15 min), 280 nm (retention time 15-45 min), and 270 nm (retention time 45-68 min), respectively. Injection volume was 10 μL at the flow rate of 1.0 mL/min. The column temperature was set at 30 ℃. Results There were good linear relationships between peak areas and contents of five components, such as paeoniflorin, naringin, hesperidin, salvianolic acid B, and tanshinone ⅡA in the ranges of 35.27-352.70 ng, 8.625-86.250 ng, 53.11-531.10 ng, 19.34-193.40 ng, and 2.142-21.420 ng. The average recoveries of five components were 100.54%, 96.78%, 97.45%, 100.25%, and 99.94% with RSD values of 0.48%, 1.07%, 1.11%, 1.18%, and 1.83%, respectively. Conclusion The established method is convenient, accurate with a satisfactory separation, and high sensitivity. It can be used to determine paeoniflorin, naringin, hesperidin, salvianolic acid B, and tanshinone ⅡA in Jiegu Pills with the same chromatogram condition.
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