健脾消癌方的HPLC-Q-TOF/mF指纹图谱分析及多指标含量测定

HPLC-Q-TOF/mF fingerprints and multi-component determination of Jianpi Xiaoai decoction

目的建立健脾消癌方的高效液相色谱(HPLC)指纹图谱和多组分含量测定方法,采用飞行时间质谱对其主要化学成分进行结构鉴定。方法制备10批健脾消癌方冻干粉,采用指纹图谱相似分析软件,对10批次样品指纹图谱的共有峰进行处理,评价不同批次样品间的质量差异;并采用高效液相色谱法串联飞行时间质谱对其主要化学成分进行结构鉴定,筛选出34种功效成分;最后对芸香柚皮苷、柚皮苷、橙皮苷、野黄芩苷、新橙皮苷、甘草酸铵6种指标性成分进行定量分析。结果健脾消癌方的HPLC指纹图谱有10个共有峰。10批健脾消癌方的HPLC指纹图谱与对照指纹图谱的相似度均≥0.900,说明指纹图谱重复性好,制备工艺较为稳定。定量分析结果表明10批健脾消癌方中芸香柚皮苷、柚皮苷、橙皮苷、野黄芩苷、新橙皮苷、甘草酸铵的质量分数范围分别为1.80~2.55、12.90~17.86、3.49~5.28、1.26~1.82、6.93~9.47、1.05~1.51 mg·g^(-1)。结论建立的健脾消癌方指纹图谱和含量测定方法分离度好、准确度高,可为该经验方制剂的研发及质量控制提供参考。

Objective To establish HPLC fingerprints and multi-component content determination method for Jianpi Xiaoai decoction,and to identify its main chemical components by time of flight mass spectrometry.Methods Ten batches of reference materials for Jianpi Xiaoai decoction were prepared.Fingerprint similarity was analyzed to process the common peaks of the fingerprints of 10 batches of samples respectively,and to evaluate the quality difference between them.The main chemical components were identified by high performance liquid chromatography tandem time of flight mass spectrometry,and 34 active components were screened out.Finally,quantitative analysis was conducted on 6 indicator components,namely brassicin,naringin,hesperidin,scutellarin,neohesperidin and ammonium glycyrrhizinate.Results There were 10 common peaks in the HPLC fingerprints of Jianpi Xiaoai decoction.The similarity between the HPLC fingerprints and the control fingerprints of the 10 batches of Jianpi Xiaoai decoction was≥0.900,indicating good reproducibility stable preparation.Quantitative analysis showed that the mass fractions of narirutin,naringin,hesperidin,baicalin,neohesperidin and ammonium glycyrrhizinate in the 10 batches of Jianpi Xiaoai decoction were 1.80 to 2.55,12.90 to 17.86,3.49 to 5.28,1.26 to 1.82,6.93 to 9.47,and 1.05 to 1.51 mg·g^(-1),respectively.Conclusion The established reference fingerprint of Jianpi Xiaoai decoction and the content determination are highly accurate and well separated,which can provide experimental basis for the development and quality control of the empirical prescription.