Key Takeaways & Executive Findings
- •• • Q-TOF-MS/MS identified 53 constituents across 8 chemical classes, with 21 tannins and 12 phenolics dominating the profile; this comprehensive mapping enables marker-based quality control beyond simple fingerprint comparison. • • Nine quantified constituents showed significantly higher average content in company B tablets versus company A (P < 0.01), indicating raw material or process disparities that directly impact therapeutic consistency. • • HCA, PCA, and OPLS-DA independently clustered the 38 batches into two distinct groups corresponding to manufacturer, with common peaks 30, 29, 16, 17, 2, 21, 10, 11, 18, 20, and 27 (e.g., procyanidin C2, B2, C1, B1, B3, gallic acid, epicatechin) as discriminatory markers. • • The 33 common peaks and 53 identified compounds establish a robust chromatographic-ms fingerprint that can serve as a reference standard for batch-to-batch consistency and cross-manufacturer quality auditing.
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Abstract
This study evaluated the quality of Fagopyri Dibotryis Rhizoma Tablets (FDRT) from two manufacturers. Eighteen batches from company A and twenty from company B were analyzed. HPLC fingerprints were established, and 33 common peaks were assigned. Quadrupole time-of-flight mass spectrometry (Q-TOF-MS/MS) identified 53 constituents, including 21 tannins, 12 phenolics, 7 flavonoids, 7 phenylpropanoid glycosides, 2 amino acids, 2 organic acids, 1 alkaloid, and 1 terpenoid. Among these, 3 phenolics (gallic acid, protocatechuic acid, protocatechualdehyde), 5 tannins (procyanidin B1, B2, B3, C1, C2), and 4 flavonoids (catechin, epicatechin, epicatechin gallate, rutin) were confirmed by reference substances. Nine constituents with good separation (excluding procyanidin C2, B2, and rutin) were quantified. The average content of these nine constituents in company B tablets was significantly higher than in company A (P < 0.01). Hierarchical cluster analysis (HCA), principal component analysis (PCA), and orthogonal partial least squares-discriminant analysis (OPLS-DA) consistently discriminated the two manufacturers into distinct clusters. Common peaks 30, 29, 16, 17, 2, 21, 10, 11, 18, 20, and 27, corresponding to procyanidin C2, B2, C1, B1, B3, gallic acid, epicatechin, etc., were identified as marker constituents responsible for quality differences. The results demonstrate significant quality divergence between FDRT from the two manufacturers.
1. Introduction
Fagopyri Dibotryis Rhizoma Tablets (FDRT) are a widely used traditional Chinese medicine preparation, yet commercial products from different manufacturers exhibit substantial compositional variability that undermines clinical reproducibility. Existing quality control protocols rely predominantly on single-marker quantification or rudimentary fingerprinting, which fail to capture the full spectrum of tannins, phenolics, and flavonoids that define the product's chemical space. This analytical gap leaves manufacturers and regulators without a reliable means to detect adulteration, raw material substitution, or process drift.
To address this bottleneck, the present study integrates HPLC fingerprinting with quadrupole time-of-flight mass spectrometry (Q-TOF-MS/MS) for comprehensive constituent identification, coupled with multivariate pattern recognition (HCA, PCA, OPLS-DA) and multi-component quantification. By analyzing 38 batches from two distinct manufacturers, the protocol not only identifies 53 constituents but also pinpoints 11 marker peaks that drive inter-manufacturer quality divergence. This dual qualitative-quantitative strategy provides a transferable framework for rigorous quality evaluation of complex herbal formulations.
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CAO Yi, HE Meng, DAI Ying, LI Yujia, YANG Junyan, DOU Zhihua (2026). Quality Evaluation of Fagopyri Dibotryis Rhizoma Tablets Based on Qualitative Analysis of HPLC Fingerprint, Q-TOF-MS/MS and Pattern Recognition Combined with Quantitative Analysis of Multi-Constituents. Chinese Traditional and Herbal Drugs. https://doi.org/10.7501/j.issn.0253-2670.2026.15.20261510
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Frequently Asked Questions
What specific chemical markers differentiate the two manufacturers' products, and what are their quantitative thresholds?
The study identified 11 common peaks (30, 29, 16, 17, 2, 21, 10, 11, 18, 20, 27) corresponding to procyanidin C2, B2, C1, B1, B3, gallic acid, epicatechin, and others as discriminatory markers. Quantification of nine constituents (excluding procyanidin C2, B2, and rutin due to poor separation) showed that company B's average content was significantly higher than company A's (P < 0.01). These markers provide concrete thresholds for quality auditing.
How robust is the HPLC fingerprint method for detecting batch-to-batch variability within a single manufacturer?
The method assigned 33 common peaks across 38 batches, with HCA, PCA, and OPLS-DA consistently clustering samples by manufacturer rather than by batch. This indicates that inter-manufacturer differences dominate over intra-manufacturer variability, making the fingerprint highly sensitive to source-specific chemical signatures. The 53 identified constituents, including 21 tannins, further anchor the method's specificity.
What are the limitations of the quantification step, and how might they affect industrial quality control?
Three constituents—procyanidin C2, B2, and rutin—were excluded from quantification due to insufficient chromatographic resolution. This leaves a gap in the quantitative profile for these flavonoids and tannins, which may still contribute to efficacy. Industrial QC labs would need to develop improved separation methods or alternative detectors (e.g., MS-based quantification) to capture these components.
Can this integrated approach be scaled for routine quality control in a manufacturing setting?
The protocol combines HPLC fingerprinting, Q-TOF-MS/MS identification, and multivariate analysis, which requires advanced instrumentation and expertise. While Q-TOF-MS/MS is not typical for routine QC, the 33 common peaks and 11 marker peaks can be translated into targeted HPLC-UV or LC-MS/MS assays. The significant content differences (P < 0.01) between manufacturers justify investment in these analytical capabilities for regulatory compliance.
What root causes might explain the significant quality divergence between company A and company B?
The study does not directly investigate root causes, but the higher content of nine constituents in company B suggests differences in raw material sourcing, extraction efficiency, or manufacturing processes. The marker compounds—procyanidins, gallic acid, epicatechin—are sensitive to oxidation and thermal degradation, implying that company A may use lower-grade rhizomes or less controlled processing. This underscores the need for supplier qualification and process validation.
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