The quality of herbal medicines (HMs) is the prerequisite for their pronounced therapeutic outcomes in clinic, and multi-component (also known as quality markers, Q-markers) quantification has been widely emphasized as a viable means for quality evaluation. Because of the chemical diversity, the quality control practices are extensively dampened by four principal technical bottlenecks, including the lack of authentic compounds, large polarity span, extensive concentration range, and signal misrecognition for those potential Q-markers. An attempt to promote the potential of LC-MS/MS is made herein to cope with those obstacles and Chinese agarwood was employed as a case study. Firstly, a home-made fraction collector was introduced to automatically fragment the entire extract into a panel of fractions-of-interest. Secondly, quantitative 1H-NMR was deployed to offset the LC-MS/MS potential towards in-depth chemical profiling each fraction, and those well-defined fractions were then pooled and combined with some accessible authentic compounds to generate the pseudo-mixed standard solution. Thirdly, serial improvements were conducted for LC-MS/MS measurements. Reversed phase LC and hydrophilic interaction LC were serially coupled in respond to the large polarity window, and online parameter optimization, response tailoring, as well as RRCEC (relative response vs. collision energy curve) matching were integrated in MS/MS domain to advance the quantitative confidences. Simultaneous determination was conducted for 26 components, in total, in Chinese agarwood after method validation. In particular, authentic compound-free quantification was achieved for eight 2-(2-phenylethyl)chromone derivatives. Above all, the strategy is a promising solution to completely tackle with the technical barriers toward Q-marker quantification-oriented quality control of Chinese agarwood, as well as other HMs.
Keywords: Authentic compound-free quantification; Chinese agarwood; Online parameter optimization; Quantitative (1)H-NMR; RPLC-HILIC; RRCEC matching.
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