一测多评法同时测定丹参配方颗粒中7个酚酸类成分

Simultaneous determination of 7 phenolic acids in Danshen formula granules by quantitatively analyze of multi-components by single-marker

目的建立一测多评法测定丹参配方颗粒中丹参素、原儿茶醛、咖啡酸、丹酚酸E、迷迭香酸、紫草酸、丹酚酸B的含量,验证其准确性及可行性。方法采用HPLC法,色谱柱为Waters Xselect HSS T3(250 mm×4.6 mm,5μm);流动相为乙腈-0.05%磷酸溶液,梯度洗脱;流速为1.2 mL·min^(-1);检测波长为286 nm。以原儿茶醛为内参物,计算其他6个成分的相对校正因子。同时采用外标法和一测多评法测定丹参配方颗粒中7个酚酸类成分的含量,比较两种方法的测定结果是否存在差异。结果丹参素、咖啡酸、丹酚酸E、迷迭香酸、紫草酸和丹酚酸B在各自质量浓度范围内与峰面积线性关系良好(r>0.999);相对校正因子分别为7.36、1.18、2.82、1.99、2.82、3.31。一测多评法与外标法测得12批样品中7个酚酸类成分的含量结果无显著差异,丹参素、咖啡酸、丹酚酸E、迷迭香酸、紫草酸、丹酚酸B相对误差分别在0.43%~0.53%、0.00%~3.70%、0.00%~0.34%、1.71%~2.01%、2.53%~2.93%、1.69%~1.73%。结论建立的一测多评法测定丹参配方颗粒中7个酚酸类成分简便稳定,可用于丹参配方颗粒的定量分析及质量控制。

Objective To establish quantitatively analyze of multi-components by single-marker(QAMS)in the simultaneous determination of tanshinol,protocatechuic aldehyde,caffeic acid,salvianolic acid E,rosmarinic acid,lithospermic acid and salvianolic acid B in Danshen formula granules,and to verify the accuracy and feasibility.Methods HPLC method was adopted.The chromatographic column Waters Xselect HSS T3(250 mm×4.6 mm,5μm)was used.The mobile phase was acetonitrile-0.05%phosphoric acid solution under gradient elution;and the flow rate was 1.2 mL·min^(-1).The detection wavelength was 286 nm.The relative correction factors of the other 6 components were calculated with protocatechuic aldehyde as the internal reference.Meanwhile,the content of the 7 phenolic acids in Danshen formula granules was determined by both the external standard method(ESM)and QAMS for further comparison.Results Tanshinol,caffeic acid,salvianolic acid E,rosmarinic acid,lithospermic acid and salvianolic acid B showed good linearity in their respective concentration ranges(r>0.999),whose relative correction factors were 7.36,1.18,2.82,1.99,2.82 and 3.31.The content of the 7 phenolic acids in 12 batches of samples determined by two assays showed no significant difference.The relative errors of tanshinol,caffeic acid,salvianolic acid E,rosmarinic acid,lithospermic acid and salvianolic acid B were 0.43%~0.53%,0.00%~3.70%,0.00%~0.34%,1.71%~2.01%,2.53%~2.93%and 1.69%~1.73%,respectively.Conclusion QAMS established for the determination of the 7 phenolic acids in Danshen formula granules is simple and stable,which can be used for the quantitative analysis and quality control of Danshen formula granules.