HPLC/qTOF-MS-oriented characteristic components data set and chemometric analysis for the holistic quality control of complex TCM preparations: Niuhuang Shangqing pill as an example.

The quality control of Da-Fu-Fang (DFF), referring to the traditional Chinese medicine (TCM) preparations comprising more than 10 TCMs, is challenging due to their extreme chemical complexity. In this study, a strategy is proposed for the holistic quality control of DFFs based on HPLC/qTOF-MS-oriented characteristic components data set (CCDS) and chemometric analysis. Niuhuang Shangqing pill (NHSQP), composed of 19 TCMs, is used to illustrate this strategy. The fingerprint profiling of NHSQP by HPLC/qTOF-MS resulted in the characterization of 190 compounds, comprising 47 unambiguously identified by reference standard comparison. A CCDS containing 60 characteristic components was constructed by analyzing the MS spectral differentiation of the crude drugs, a laboratory-made NHSQP powder, and negative control preparations. With the established CCDS, it was possible to simultaneously monitor 16 out of the 19 drugs involved in NHSQP. Subsequently, 26 NHSQP samples from different vendors were evaluated by the qualitative and semi-quantitative analyses of their LC/MS fingerprint data. The 60 characteristic components were detected in all of the NHSQP samples, which demonstrated their authenticity. When compared with the standard sample No. 3, however, 15 of the NHSQP samples exhibited inferior quality. Samples No. 21 and No. 13 differed significantly based on a PCA score plot, and the components responsible for the differentiation were confirmed to originate from different TCMs. This strategy is a powerful and easy method to implement and provides a potential approach to establishing the holistic quality control of complex TCM preparations.