Screening Synthetic Adulterants from Herbal and Dietary Supplements (HDS) Using the Natural Products Application Solution with UNIFI

Significance of the Topic

Adulteration of herbal and dietary supplements with undeclared synthetic drugs presents significant health and regulatory challenges. Reports of severe adverse events, including fatal outcomes, underscore the need for robust analytical approaches. High‐performance liquid chromatography coupled with high‐resolution mass spectrometry (LC–MS) is a gold‐standard technique for detecting trace synthetic adulterants in complex botanical matrices, but streamlined, user‐friendly workflows are essential to improve throughput and consistency.

Objectives and Overview of the Study

This study demonstrates a turnkey solution for rapid screening and confirmation of synthetic adulterants in a commercial anti‐inflammatory herbal supplement. Using the Natural Products Application Solution powered by UNIFI software and a dedicated Synthetic Adulterants Library, the workflow integrates sample preparation, data acquisition, automated component identification, fragment ion verification, and report generation into a single, efficient process.

Methodology

• Sample preparation: 1 g of powdered supplement extracted in 10 mL LC–MS grade methanol, sonicated for 20 min, centrifuged at 4472 g for 5 min, 250× dilution, 1 µL injection.
• Chromatographic separation: Waters ACQUITY UPLC I-Class with HSS T3 column (2.1×100 mm, 1.8 µm) at 40 °C; 17 min gradient from 2% to 100% acetonitrile (0.1% formic acid).
• Mass spectrometry: Xevo G2-XS QTof operated in ESI+ and ESI– with MS E data‐independent acquisition; scan range 50–1500 Da; low collision energy 6 eV, high collision energy ramp 10–40 eV; resolution mode with lock mass correction.
• Data processing: UNIFI Adulterant Screening Application employing seven preset workflows linked to the Synthetic Adulterants Library for automated peak picking, library matching, fragment verification, and report generation.

Instrumentation Used

• Waters ACQUITY UPLC I-Class System with Flow Through Needle (FTN) sample manager
• Waters Xevo G2-XS QTof Mass Spectrometer
• Natural Products Application Solution with UNIFI software
• Catechin standard mixture for system suitability testing

Main Results and Discussion

Analysis of a street‐vendor herbal capsule revealed two nonsteroidal anti‐inflammatory drug (NSAID) adulterants: phenylbutazone (direct library match) and its metabolite oxyphenbutazone (identified via structural elucidation). Phenylbutazone met parent mass and diagnostic fragment criteria within 2 mDa mass error. A high‐abundance unknown component at 8.29 min was subjected to elemental composition determination (C19H20N2O3, i-FIT 99.9%), online ChemSpider search, and MassFragment prediction of MS/MS fragments, confirming oxyphenbutazone. Automated review templates categorized “Good Matches,” “Tentative Matches,” and “No Match High Intensity,” enabling focused confirmation workflows and rapid report generation.

Benefits and Practical Applications of the Method

• Fully integrated, sample‐to‐report pipeline reduces manual intervention, operator expertise, and processing time.
• Dedicated Synthetic Adulterants Library enhances detection of common and emerging synthetic drugs.
• Automated fragment verification minimizes false positives and supports confident identification.
• Scalable workflow adaptable for routine quality control, contract testing, and regulatory monitoring.

Future Trends and Potential Applications

• Expansion of adulterant libraries to include novel synthetic analogues and region‐specific compounds.
• Integration of machine learning models to prioritize unknown high‐intensity peaks for structural elucidation.
• Application of similar workflows to other complex natural product matrices (e.g., botanical extracts, traditional medicines).
• Cloud‐based data sharing and collaborative annotation to support global surveillance of adulterated products.

Conclusion

The Natural Products Application Solution with UNIFI Adulterant Screening Application offers a robust, high‐throughput approach for detecting and confirming synthetic adulterants in herbal supplements. The combination of LC–MS data‐independent acquisition, a comprehensive adulterant library, and automated processing workflows delivers rapid, reliable results with minimal expert input, meeting the demands of modern quality assurance and regulatory environments.

References

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