基于指纹图谱、量值传递及化学计量学的薏苡竹叶散质量评价

Research on Quality Evaluation of Yiyi-Zhuye Powders Based onFingerprint, Quality Value Transfer and Chemometrics

建立高效液相指纹图谱进行外部质量控制,结合化学计量学探究内部质量影响因素,通过量值传递规律确定制备工艺稳定性,全面完善薏苡竹叶散(YZP)质量评价系统。利用《中药色谱指纹图谱相似度评价系统》(2012.130723版本)绘制15批YZP指纹图谱并评价相似度;选择Origin 2019b 64Bit进行聚类分析(CA),利用SIMCA 14.1进行主成分分析(PCA)和正交偏最小二乘判别分析(OPLS-DA),获得导致质量差异的主要成分;测定15批淡竹叶药材和YZP中荭草苷和异荭草苷的含量,探究样品制备过程中的量值传递规律。结果表明,15批YZP指纹图谱得到21个共有峰,指认了6种成分,分别为9号峰(异荭草苷)、10号峰(荭草苷)、13号峰(牡荆素)、14号峰(异牡荆素)、15号峰(连翘酯苷A)和20号峰(连翘苷),相似度在0.956~0.995之间,符合相关规定;CA结果显示,15批YZP被分为两类,PCA共得到3个主成分,累计贡献率82.4%,OPLS-DA得出10个贡献率较大成分,包括已指认出的9号峰(异荭草苷)、13号峰(牡荆素)和20号峰(连翘苷),有利于进一步质量评价;15批淡竹叶饮片中荭草苷、异荭草苷的质量分数为0.2156%~0.9923%、0.530%~2.052%,15批YZP中荭草苷、异荭草苷的质量分数为0.022%~0.112%、0.065%~0.312%,饮片-YZP中荭草苷、异荭草苷转移率为78.41%~119.54%、74.57%~127.96%,转移率皆在平均值±30%范围内,未出现离散值,说明制备工艺较稳定。本文建立了HPLC指纹图谱结合多指标含量测定方法,有效控制YZP外部质量,通过化学计量学确定了影响质量的内部因素,转移率稳定确定制备工艺稳定可靠,为YZP全面质量评价奠定基础。

High performance liquid chromatography(HPLC)fingerprints are established for external quality control,internal quality influencing factors are explored in combined with chemometrics,the stability of the preparation process is determined by the law of quantity value transfer,and the quality evaluation system of Yiyi-Zhuye Powder(YZP)is comprehensively improved.The fingerprints of 15 batches of YZP are mapped and evaluated by similarity Evaluation System of TCM Chromatographic Fingerprint(2012.130723 version);Origin 2019b 64Bit is selected for cluster analysis(CA),and SIMCA 14.1 is used for principal component analysis(PCA)and orthogonal partial least squares discriminant analysis(OPLS-DA)to obtain the main components that causes the quality difference;The contents of orientin and isoorientin in 15 batches of Lophatherum gracile and YZP are determined to investigate the law of quality value transfer in the process of sample preparation.A total of 21 peaks are obtained from 15 batches of YZP,of which 6 peaks are identified as peak 9(isoorientin),peak 10(orientin),peak 13(vitexin),peak 14(isovitexin),peak 15(forsythiolate glycoside A)and peak 20(forsythiin).The similarity is between 0.956 and 0.995,which meets the relevant regulations.CA results show that 15 batches of YZP are divided into two categories.PCA obtains 3 principal components with a cumulative contribution rate of 82.4%,and OPLS-DA obtains 10 components with a large contribution rate,including peak 9,peak 13 and peak 20,which is conducive to further quality evaluation.The content ranges of orientin and isoorientin in 15 batches of Lophatherum Herb are 0.2156%~0.9923%and 0.530%~2.052%,while the content ranges of orientin and isoorientin in 15 batches of YZP are 0.022%~0.112%and 0.065%~0.312%.The transfer rates are 78.41%~119.54%and 74.57%~127.96%,respectively,and all are in the mean±30%range,indicating that the preparation process is stable.A combined HPLC fingerprint and multi-index content determination method has been established to effectively control the external quality of YZP,and the internal factors affecting the quality are determined by chemometrics.The stable transfer rate determines that the preparation process is stable and reliable,which lays a foundation for the comprehensive quality evaluation of YZP.