高效液相色谱法测定陈香舒胃片中大黄素、大黄酚、大黄素甲醚的含量

摘要

Objective To establish a method for the determination of emodin,chrysophanol and rhubarb in Chenxiangshu stomach tablets.Methods HPLC was used.The column was SHIMAUZU VP-OD (250mm × 4.5 mm,5 μm);mobile phase:methanol (A)-0.1％ phosphoric acid solution (B),gradient elution;flow rate:1.0 ml/min;detection wavelength:254 nm;column temperature:30 ℃;injection volume 20 μl.Results The emodin,chrysophanol,and rhein were linear in the range of 0.518～4.144 μg/ml,0.372～2.976 μg/ml,and 1.109～8.872 μg/ml,respectively;the quantification limits were 1.24 ng,0.53 ng,and 1.55 ng,respectively;the detection limits were 0.42 ng,0.19 ng,and 0.55 ng,respectively.The average recovery rate of emodin was 99.92％,and RSD was 0.13％;the average recovery rate of chrysophanol was 99.98％,and RSD was 0.15％;the average recovery rate of rhubarb was 99.95％,and the RSD was 0.18％.Conclusions The method developed in this study is simple,reproducible,high in recovery,and stable in stability.It can be used for quality control of Chenxiangshu stomach tablets.%目的 建立陈香舒胃片中大黄素、大黄酚、大黄素甲醚含量的测定方法.方法 采用高效液相色谱,色谱柱为:SHIMAUZU VP-OD(250.0 mm×4.5 mm,5μm);流动相:甲醇(A)-0.1％磷酸溶液(B),梯度洗脱;流速:1.0 ml/min;检测波长:254 nm;柱温:30℃;进样量20μl.结果 大黄素、大黄酚、大黄素甲醚分别在0.518～4.144 μg/ml、0.372～2.976μg/ml、1.109～8.872μg/ml范围内线性关系良好;定量限分别为1.24 ng、0.53 ng、1.55 ng;检测限分别为0.42 ng、0.19 ng、0.55 ng;大黄素平均加样回收率为99.92％,RSD为0.13％;大黄酚平均加样回收率为99.98％,RSD为0.15％;大黄素甲醚平均加样回收率为99.95％,RSD为0.18％.结论 本研究建立的方法简便易行、重复性好、回收率高、稳定性强,可用于陈香舒胃片的质量控制.