[关键词]
[摘要]
目的 建立一种RP-HPLC同时测定益肾排毒丸中毛蕊异黄酮葡萄糖苷、大黄素和大黄素甲醚等3种成分含量的方法及指纹图谱。方法 采用Agilent TC-C18色谱柱(250 mm×4.6 mm,5 μm),流动相为乙腈(A)-0.2%甲酸溶液(B)梯度洗脱(0~20 min,20%~40% A;20~30 min,40% A;30~35 min,90% A;35~40 min,20% A),体积流量1.0 mL/min,柱温30℃,检测波长260 nm。结果 毛蕊异黄酮葡萄糖苷、大黄素和大黄素甲醚分离度较好,且在各自浓度范围内呈现出良好的线性关系,r=0.999 2;精密度可靠(RSD为0.63%~0.74%);样品在12 h内稳定;方法重复性良好(RSD为1.39%~2.00%);3种成分的平均加样回收率分别为100.3%、100.5%、103.2%,RSD均小于2.0%。采用HPLC可准确有效测出益肾排毒丸中有效成分的含量。指纹图谱研究得共有峰32个,指认了其中6个成分,益肾排毒丸各批次间一致性较好,质量相对稳定。结论 该方法简便易行、稳定可靠,可更好用于益肾排毒丸的质量控制。
[Key word]
[Abstract]
Objective To establish an RP-HPLC method for simultaneous determination of the contents of three ingredients (calycosin glycoside,emodin,physcion) and fingureprint in Yishen Paidu Pills.Methods The analysis was performed on Agilent TCC18 column (250 mm×4.6 mm,5 μm) with the mobile phase of acetonitrile (A) and 0.2% formic acid (B) in a liner gradient mode as follows:0-20 min,20%-40% A;20-30min,40% A;30-35 min,90% A;35-40 min,20% A.The flow rate was 1.0 mL/min.The column temperature was 30℃ and the detective wavelength was at 260 nm.Results The standard curves of three ingredients showed good linearity in their concentration ranges with r=0.999 2.Precision was reliable (RSD in 0.63%-0.74%).Samples were stable in 12 h and the repeatability of method was excellent (RSD in 1.39%-2.0%).The average recovery of the three ingredients were 100.3%,100.5% and 103.2%,respectively with RSD less than 2.0%.The contents of three ingredients in Yishen Paidu Wan can be determined accurately and effectively by HPLC.Fingerprints study of Yishen Paidu Pills indicated that they have good consistency among different batches and the quality were relatively stable.Conclusion The method is rapid,simple and accurate,and can be better applied for the quality control of Yishen Paidu Pills.
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[基金项目]
国家自然科学基金(81803799);中央高校基本科研业务费专项资金(2017KFYXJJ252);湖北省自然科学基金(2017CFB273)