复方独活益肾合剂质量标准提升研究

Improvement of the Quality Standard of Compound Duhuo Yishen Mixture

目的提升复方独活益肾合剂的质量标准。方法采用薄层色谱法对制剂中独活、白芍及秦艽进行定性鉴别;采用高效液相色谱法测定制剂中芍药苷的含量,色谱柱为Welch ZapchromTM C18柱(250 mm×4.6 mm,5μm),流动相为乙腈(A)-0.1%磷酸溶液(B),梯度洗脱(0~16 min时15%A,16~25 min时15%A~70%A,25~35 min时70%A~15%A),流速为1.0 m L/min,检测波长为230 nm,柱温为30℃,进样量为5μL。结果独活、白芍、秦艽的薄层色谱图斑点清晰,分离度好,专属性强,阴性对照无干扰。芍药苷进样量在36.10~541.50μg范围内与峰面积线性关系良好;精密度、稳定性、重复性试验结果的RSD均小于2%(n=6);平均加样回收率为101.54%,RSD为1.22%(n=6)。结论所建立的方法准确可靠,专属性强,稳定性及重复性均较好,可用于提升复方独活益肾合剂的质量标准。

Objective To improve the quality standard of Compound Duhuo Yishen Mixture.Methods Thin-layer chromatography(TLC)method was used for the qualitative identification of Radix Angelicae Pubescentis,Radix paeoniae alba and Radix Gentianae Macrophyllae in Duhuo Yishen Mixture.High-performance liquid chromatography method(HPLC)was used for the content determination of paeoniflorin in Duhuo Yishen Mixture,the chromatographic column was Welch ZapchromTM C18 column(250 mm×4.6 mm,5μm),the mobile phase was acetonitrile(A)-0.1%phosphoric acid solution(B)with gradient elution(0-16 min,15%A;16-25 min,15%A-70%A;25-35 min,70%A-15%A),the flow rate was 1.0 m L/min,the detection wavelength was 230 nm,the column temperature was30℃,and the injection volume was 5μL.Results The TLC spots of Radix Angelicae Pubescentis,Radix paeoniae alba and Radix Gentianae Macrophyllae were clear with good resolution and strong specificity,and the negative control had no interference.The linear range of paeoniflorin was 36.10-541.50μg.The RSDs of precision,stability and repeatability tests were less than 2%(n=6).The average recovery of paeoniflorin was 101.54%with RSD of 1.22%(n=6).Conclusion The established method is accurate,reliable,specific,stable and reproducible,which can be used to improve the quality standard of Compound Duhuo Yishen Mixture.