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[摘要]
目的 建立高效液相色谱梯度洗脱法同时测定心无忧片中洋川芎内酯H、洋川芎内酯I、洋川芎内酯A、藁本内酯、丹参素、丹酚酸B和丹参酮ⅡA的方法。方法 采用Hydrosphere C18色谱柱(250 mm×4.6 mm,5 μm);流动相A:甲醇–乙腈(2:1),流动相B:0.2%冰醋酸溶液,梯度洗脱(0~11 min,45.0% A;11~26 min,45.0%→68.0% A;26~39 min,68.0%→82.0% A;39~45 min,82.0%→45.0% A);检测波长:280 nm;体积流量:0.9 mL/min;柱温:30℃;进样量为10 μL。结果 洋川芎内酯H、洋川芎内酯I、洋川芎内酯A、藁本内酯、丹参素、丹酚酸B和丹参酮ⅡA的线性范围分别为2.08~41.60 μg/mL(r=0.999 3),3.36~67.20 μg/mL(r=0.999 8),4.29~85.80 μg/mL(r=0.999 9),6.26~125.20 μg/mL(r=0.999 6),3.49~69.80 μg/mL(r=0.999 2),49.08~981.60 μg/mL(r=0.999 7),7.17~143.40 μg/mL(r=0.999 5);平均加样回收率分别为96.81%、98.19%、99.24%、98.93%、97.39%、100.19%、98.63%,RSD值分别为1.51%、1.24%、0.98%、1.12%、0.84%、0.74%、1.44%。结论 建立的HPLC梯度洗脱法同时测定心无忧片中心无忧片中洋川芎内酯H、洋川芎内酯I、洋川芎内酯A、藁本内酯、丹参素、丹酚酸B和丹参酮ⅡA7个成分的测定方法,供试品溶液处理简便,溶液稳定性好,检测方法快捷、准确、灵敏度高,为心无忧片质量标准的提高提供了参考。
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[Abstract]
Objective To develop HPLC gradient elution method for simultaneous determination of senkyunolide H, senkyunolide I, senkyunolide A, ligustilide, danshensu, salvianolic acid B, and tanshinoneⅡA in Xinwuyou Tablets. Methods The determination was carried out on Hydrosphere C18 column (250 mm×4.6 mm, 5 μm). The mobile phase was methanol-acetonitrile (2:1) and 0.2% acetic acid glacial solution with gradient elution. The elution procedures were as following:0 — 11 min with 45.0% A, 11 — 26 min with 45.0%→68.0% A, 26 — 39 min with 68.0%→82.0% A, and 39 — 45 min with 82.0%→45.0% A. The detection wavelengths were set at 280 nm. The flow rate was 0.9 mL/min, temperature of column was set at 30℃, and volume of injection was 10 μL. Results Senkyunolide H, senkyunolide I, senkyunolide A, ligustilide, danshensu, salvianolic acid B, and tanshinoneⅡAhad good linearities in the range of 2.08 — 41.60 μg/mL (r=0.999 3), 3.36 — 67.20 μg/mL (r=0.999 8), 4.29 — 85.80 μg/mL (r=0.999 9), 6.26 — 125.20 μg/mL (r=0.999 6), 3.49 — 69.80 μg/mL (r=0.999 2), 49.08 — 981.60 μg/mL (r=0.999 7), and 7.17 — 143.40 μg/mL (r=0.999 5), respectively. The average recoveries were 96.81%, 98.19%, 99.24%, 98.93%, 97.39%, 100.19%, and 98.63%, respectively. And the corresponding RSD values were 1.51%, 1.24%, 0.98%, 1.12%, 0.84%, 0.74%, and 1.44%, respectively. Conclusion The established method of HPLC gradient elution method for simultaneous determination of senkyunolide H, senkyunolide I, senkyunolide A, ligustilide, danshensu, salvianolic acid B, and tanshinone ⅡA in Xinwuyou Tablets is simple for the solution treatment, stable for the solution, and fast for the detection method. The method is accurate and sensitive which can be applied to reference for the quality control of Xinwuyou Tablets.
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