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Chemical profiling and quantification of Chinese medicinal formula Huang-Lian-Jie-Du decoction, a systematic quality control strategy using ultra high performance liquid chromatography combined with hybrid quadrupole-orbitrap and triple quadrupole mass spectrometers

Journal name:Journal of Chromatography A
Document No.:Volume 1321, 20 December 2013, Pages 88–99, doi:10.1016/j.chroma.2013.10.072
Document URL: http://www.sciencedirect.com/science/article/pii/S0021967313016919
Date publication:20 December 2013


To clarify and quantify the chemical profiling of Huang-Lian-Jie-Du decoction (HLJDD) rapidly, a feasible and accurate strategy was developed by applying high speed LC combined with hybrid quadrupole-orbitrap mass spectrometer (Q-Exactive) and UHPLC–triple quadruple mass spectrometer (UHPLC–QqQ MS). 69 compounds, including iridoids, alkaloids, flavonoids, triterpenoid, monoterpene and phenolic acids, were identified by their characteristic high resolution mass data. Among them, 18 major compounds were unambiguously detected by comparing with reference standards. In the subsequent quantitative analysis, 17 representative compounds, selected as quality control markers, were simultaneously detected in 10 batches of HLJDD samples by UHPLC–QqQ MS. These samples were collected from four different countries (regions). Icariin, swertiamarin and corynoline were employed as internal standards for flavonoids, iridoids and alkaloids respectively. All the analytes were detected within 12 min. Polarity switching mode was used in the optimization of multiple reaction monitoring (MRM) conditions. Satisfactory linearity was achieved with wide linear range and fine determination coefficient (r2 > 0.9990). The relative standard deviations (RSD) of inter- and intra-day precisions were less than 5.0%. This method was also validated by repeatability, stability (8 h) and recovery, with respective RSDs less than 4.6%, 5.0% and 6.3%. This research established a high sensitive and efficient method for the integrating quality control, including identification and quantification of Chinese medicinal formulas.


Coptisine (13), epiberberine (9) and jatrorrhizine (14) were purchased from Chengdu Herbpurify Co. Ltd. (Chengdu, China). ...

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