UPLC-ELSD指纹图谱结合化学计量学方法用于骨刺片的质量控制

Quality control of Guci tablets using UPLC-ELSD fingerprint analysis coupled with chemometrics

建立了骨刺片UPLC-ELSD指纹图谱分析方法，色谱柱为WatersAcquityUPLCBEHC18柱（2．1mm×100mm，1．7μm），以0．1％甲酸水溶液一乙腈为流动相梯度洗脱，柱温30℃，流速0．3mL·min^-1，进样体积3μL，ELSD气体压力0．28MPa，漂移管温度60℃，增益400。采用该方法测定6个厂家生产的39批骨刺片，并采用ChemPattern软件进行分析。以75％以上样品中存在的色谱峰作为共有峰筛选条件，确定了30个共有蜂，采用RRLC-MS／MS联用技术对其中19个共有峰进行指认，并对其中16个成分采用对照品比对的方式进行确证。样品与共有模式的相似度为0．47～0．98，表明不同厂家生产的骨刺片的质量相差较大，此外，对色谱数据进行主成分分析和聚类分析，阐明不同厂家制剂的主要差异性成分，结合这些成分的药材来源，推测部分厂家在三七、白芍和威灵仙投料方面可能存在问颢．从而为骨刺片总体质量控制和标准提高提供参考。

Uhra-performance liquid chromatography-evaporative light scattering detection （UPLC-ELSD） fingerprint analysis meth- od was established tor quality control of Guei tablets. Chromatographic separation was performed on Waters Acquity UPLC BEH Cis col- umn （2.1 mm × 100 mm, 1.7 μm） at 30 ℃ of column temperature. Acetonitrile-0.1% formic acid solution was adopted as mobile phase for gradient elution. The flow rate was set at 0.3 mL,min^-11, and the injection volume was 3 μL. Detection was carried out on an ELSD with a nitrogen pressure of 0.28 MPa, drift tube temperature of 60 ℃, and gain of 400. A total of 39 batches of samples pro- duced by six manufacturers were measured by using the above method and the data were analyzed by ChemPattern software. The peak present in more than 75% of the samples was defined as a common peak, and 30 common peaks were determined. Among them, 19 peaks were identified by rapid resolution liquid chromatography/tandem mass spectrometry （RRLC-MS/MS） method, 16 of which were confirmed by reference substances. The similarity of the tested samples was 0.47-0.98, suggesting that the quality of the samples from different manufacturers varied greatly. Furthermore, principal component analysis （PCA） and hierarchical analysis （HCA） were per- formed to clarify the main different components in samples. The results indicated that there might be some feeding problems about Pae- oniae Radix Alba, Notogiilseng Radix et Rhizoma, and Clematidis Radix et Rhizoma in a few manufacturers. This study provided some evidenees for the overall quality control of Guci tablets, as well as its quality standard improvements.