摘要
目的采用HPLC梯度洗脱法同时测定沉香化滞丸中沉香四醇、柚皮苷、橙皮苷、新橙皮苷、和厚朴酚、大黄素、厚朴酚、木香烃内酯、去氢木香内酯、大黄酚、大黄素甲醚11种成分。方法采用Thermo Syncronis C18色谱柱(250 mm×4.6 mm,5μm),流动相为水-乙腈,梯度洗脱:0～10 min,20%乙腈;10～20 min,20%～40%乙腈;20～24 min,40%乙腈;24～26 min,40%～52%乙腈;26～30 min,52%乙腈;30～31 min,52%～90%乙腈;31～35 min,90%乙腈;35～40 min,90%～100%乙腈;40～43min,100%乙腈;43～45min,100%～20%乙腈;检测波长215nm,体积流量1.0m L/min,柱温30℃,进样量20μL。结果各成分在43 min内分离良好,沉香四醇、柚皮苷、橙皮苷、新橙皮苷、和厚朴酚、大黄素、厚朴酚、木香烃内酯、去氢木香内酯、大黄酚、大黄素甲醚的线性范围分别为1.4～13.6、10.0～200.0、31.5～315.0、1.0～120.1、1.8～50.6、0.93～10.1、1.8～30.0、0.2～40.3、1.8～18.1、1.7～25.0、0.45～10.70μg/mL;样品中各成分的平均回收率均在98.90%～100.87%;11种成分精密度RSD在0.55%～1.54%;供试品溶液在30 h内稳定性良好,RSD在0.75%～1.94%;重复性RSD在0.39%～1.73%。6批次样品中沉香四醇、柚皮苷、橙皮苷、新橙皮苷、和厚朴酚、大黄素、厚朴酚、木香烃内酯、去氢木香内酯、大黄酚、大黄素甲醚质量分数分别为92.0～201.0、511.5～9 033.0、5 475.0～12 635.5、54.5～5 095.5、192.0～2 137.5、117.0～391.5、106.5～1 281.5、13.0～136.5、93.5～199.0、177.0～1 207.0、33.5～251.5μg/g。结论本方法准确、快速、简便,重复性好,精密度高,适用于沉香化滞丸中多种活性成分的定量分析。
Objective To develop an HPLC method for simultaneous determination of the eleven constituents(agaric-alcohol,naringin, hesperidin, neohesperidin, honokiol, emodin, magnolol, costunolide, dehydrocostus, chrysophanol, and physcion) in Chenxiang Huazhi Pills(CHP) by HPLC with gradient elution. Methods The chromatographic separation was performed on an Thermo Syncronis C18 column(4.6 mm × 250 mm, 5 μm) which was operated at 30 ℃. The mobile phase was a linear gradient prepared from water(A) and acetonitrile(B). The linear gradient elution program was programmed as follows: 0-10 min, 20%acetonitrile;10-20 min, 20%-40% acetonitrile;20-24 min, 40% acetonitrile;24-26 min, 40%-52% acetonitrile;26-30 min,52% acetonitrile;30-31 min, 52%-90% acetonitrile;31-35 min, 90% acetonitrile;35-40 min, 90%-100% acetonitrile;40-43 min, 100% acetonitrile;43-45 min, 100%-20% acetonitrile. The flow rate was 1 mL/min and the detection wavelength was 215 nm.Results The analysis permitted very good separation of eleven constituents within 43 min. A good linear relationship between the peak area and the injection volume was obtained. The ranges of the eleven constituents were 1.4-13.6, 10.0-200.0, 31.5-315.0,1.0-120.1, 1.8-50.6, 0.93-10.1, 1.8-30.0, 0.2-40.3, 1.8-18.1, 1.7-25.0, and 0.45-10.70 μg/mL. The average recoveries of eleven constituents in the samples were in the range of 98.90%-100.87%. The precision RSD of the peak areas of the 11 components ranged from 0.55%-1.54%;Eleven components had good stability within 30 h, and the concentration RSD of each component ranged from 0.75% to 1.94%;The repeatability RSD of each component ranged from 0.39% to 1.73%. The content of agaric-alcohol, naringin,hesperidin, neohesperidin, honokiol, emodin, magnolol, costunolide, dehydrocostus, chrysophanol, and physcion in six batches were92.0-201.0, 511.5-9 033.0, 5 475.0-12 635.5, 54.5-5 095.5, 192.0-2 137.5, 117.0-391.5, 106.5-1 281.5, 13.0-136.5,93.5-199.0, 177.0-1 207.0, and 33.5-251.5 μg/g, respectively. Conclusion The method is accurate, rapid and simple with high sensitivity, precision and repeatability, which has been successfully applied as an effective tool for the multicomponent analysis of CHP.
作者
段芳芳
江雯雯
吴珊湖
刘佳卓
杜明荦
苏梦翔
DUAN Fang-fang;JIANG Wen-wen;WU Shan-hu;LIU Jia-zhuo;DU Ming-luo;SU Meng-xiang(School of Pharmacy,China Pharmaceutical University,Nanjing 210009,China;Henan Provincial Institute of Food and Drug Control,Zhengzhou 450003,China)
出处
《中草药》
CAS
CSCD
北大核心
2019年第9期2094-2100,共7页
Chinese Traditional and Herbal Drugs
基金
国家级大学生创新创业训练计划项目(201410316060)
大学生创新药物研制能力提高项目(J1030830)
