基于多波长-UPLC指纹图谱及多成分含量测定对胡黄连总苷胶囊的质量控制研究

Research on quality control of Picrorhiza scrophulariiflora total glycosides capsules based on multi-wavelength-UPLC fingerprint and multi-component content determination

目的建立多波长-超高效液相色谱(UPLC)测定胡黄连总苷胶囊指纹图谱及多成分的含量测定方法。方法采用ACQUITY UPLC BEH C8色谱柱(2.1 mm×100 mm,1.7μm),流动相为0.1%甲酸-乙腈梯度洗脱,检测波长为0~6 min 260 nm、6~10 min 300 nm、10~22 min 270 nm,流速为0.35 ml/min,柱温30℃。结果在建立的指纹图谱中共标定了16个共有峰,并用对照品指认11个共有峰,指纹图谱相似度均≥0.99;测定其中5个成分(草夹竹桃苷、香草酸、胡黄连苷Ⅰ、胡黄连苷Ⅱ、胡黄连苷Ⅳ)的含量测定结果在范围内呈线性相关;平均加样回收率97.60%~103.90%,RSD为1.79%~2.14%;精密度、重复性、稳定性实验RSD均≤1.45%。结论该方法重复性好、准确度高,可用于胡黄连总苷胶囊的质量控制研究。

Objective To establish a multi-wavelength ultra-high performance liquid chromatography(UPLC)method for the determination of the fingerprint and the content of multi-components of Picrorhiza scrophulariiflora total glycosides capsules.Methods ACQUITY UPLC BEH C8 column(2.1 mm×100 mm,1.7μm)was used,and the mobile phase was 0.1%formic acid-acetonitrile gradient elution.The detection wavelength was 0-6 min 260 nm,6-10 min 300 nm,and 10-22 min 270 nm,the flow rate was 0.35 ml/min,and the column temperature was 30℃.Results 16 common peaks were identified in the established fingerprint,and 11 common peaks were identified by reference substance,and the similarity of fingerprint were all≥0.99.The content of 5 components(oleander glycoside,vanillic acid,picrosideⅠ,picrosideⅡ,picrosideⅣ)was determined linearly within the range.The average sample addition recovery rate was 97.60%-103.90%,and RSD was 1.79%-2.14%.The RSD of precision,repeatability and stability tests were all≤1.45%.Conclusion The method is reproducible and accurate,and can be used for the quality control research of Picrorhiza scrophulariiflora total glycosides capsules.