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[摘要]
目的 建立同时测定心脑康片中11种成分(丹参酮ⅡA、葛根素、β-蜕皮甾酮、甘草苷、芍药苷、斯皮诺素、阿魏酸、山柰素、大黄素、细叶远志皂苷和23-乙酰泽泻醇B)的HPLC分析方法。方法 采用HPLC法测定心脑康片中丹参酮ⅡA、葛根素、β-蜕皮甾酮、甘草苷、芍药苷、斯皮诺素、阿魏酸、山柰素、大黄素、细叶远志皂苷和23-乙酰泽泻醇B。色谱柱为InertSustain C18柱(250 mm×4.6mm,5μm);甲醇-乙腈(1:1,A)-0.1%磷酸水溶液(B)为流动相,梯度洗脱:0~10.0 min,80% B;10.0~20.0 min,80%~70% B;20.0~35.0 min,70%~50% B;35.0~50.0 min,50%~30% B;体积流量0.9mL/min;柱温40℃;进样量10μL。结果 丹参酮ⅡA、葛根素、β-蜕皮甾酮、甘草苷、芍药苷、斯皮诺素、阿魏酸、山柰素、大黄素、细叶远志皂苷和23-乙酰泽泻醇B分离度良好,分别在28.24~282.42、15.89~158.90、20.53~205.26、4.09~40.94、12.08~120.76、40.03~404.30、4.08~40.75、2.13~21.25, 7.91~79.14、20.30~202.96、4.10~40.96μg/mL线性关系良好,r均大于0.9990,平均加样回收率为98.15%~101.84%(RSD在0.62%~1.71%)。6批样品中丹参酮ⅡA、葛根素、β-蜕皮甾酮、甘草苷、芍药苷、斯皮诺素、阿魏酸、山柰素、大黄素、细叶远志皂苷和23-乙酰泽泻醇B分别在0.870~0.887、6.321~6.329、0.857~0.866、0.171~0.179、0.369~0.377、2.128~2.136、0.088~0.099、0.148~0.155、0.113~0.121、0.371~1.380、0.101~0.109 mg/g。结论 本法快速、灵敏度高、准确度高、专属性好,为心脑康片的质量控制提供依据。
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[Abstract]
Objective To establish a method of HPLC for the simultaneous determination of eleven ingredients (tanshinone ⅡA, puerarin, β-ecdysone, liquiritin, paeoniflorin, spinosin, ferulic acid, kaempferide, emodin, tenuifolin, and 23-acetate alisol B) in Xinnaokang Tablets. Methods The contents of tanshinone ⅡA, puerarin, β-ecdysone, liquiritin, paeoniflorin, spinosin, ferulic acid, kaempferide, emodin, tenuifolin, and 23-acetate alisol B were determined by HPLC. Separation was performed on an InertSustain C18 column (250 mm×4.6 mm, 5 μm); Mobile phase was methanol-acetonitrile (1:1, A)-0.1% phosphoric acid (B), gradient elution:0-10.0 min, 80% B; 10.0-20.0 min, 80%-70% B; 20.0-35.0 min, 70%-50% B; and 35.0-50.0 min, 50%-30% B; Flow rate was 0.9 mL/min; Column temperature was 40℃; Injection volume was 10 μL. Results The separations of tanshinone ⅡA, puerarin, β-ecdysone, liquiritin, paeoniflorin, spinosin, ferulic acid, kaempferide, emodin, tenuifolin, and 23-acetate alisol B were good.The linear ranges were good,28.24-282.42, 15.89-158.90, 20.53-205.26, 4.09-40.94, 12.08-120.76,40.03-404.30, 4.08-40.75, 2.13-21.25, 7.91-79.14, 20.30-202.96, and 4.10-40.96μg/mL for tanshinone ⅡA, puerarin, β-ecdysone, liquiritin, paeoniflorin, spinosin, ferulic acid, kaempferide, emodin, tenuifolin,and 23-acetate alisol B, respectively, with the correlation r> 0.999 0. The extraction recoveries varied from 98.15% to 101.84% (RSD varied from 0.62% to 1.71%). The contents of tanshinone ⅡA, puerarin, β-ecdysone, liquiritin, paeoniflorin, spinosin, ferulic acid, kaempferide, emodin, tenuifolin,and 23-acetate alisol Bwere 0.870-0.887,6.321-6.329, 0.857-0.866, 0.171-0.179, 0.369-0.377, 2.128-2.136, 0.088-0.099, 0.148-0.155, 0.113-0.121,0.371-1.380, and 0.101-0.109 mg/gin six batches of samples, respectively. Conclusion This method is rapid and has high sensitivity, high accuracy, and good specificity,which can provide the basis for the quality control of Xinnaokang Tablets.
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