HPLC法同时测定心脑康片中11种成分

Simultaneous determination of eleven ingredients in Xinnaokang Tablets by HPLC

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Inert Sustain C18柱(250 mm×4.6 mm,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0.9 m L/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/m L线性关系良好,r均大于0.999 0,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。

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 Inert Sustain C18column(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 m L/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—40.96 μg/m L 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 B were 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/g in 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.