EVALUATION OF AN OPEN AMBIENT IONISATION SOURCE COUPLED TO A PORTABLE MASS DETECTOR AS A TOOL FOR THE RAPID DETECTION OF UNDECLARED ACTIVE INGREDIENT(S) IN ONLINE HEALTH SUPPLEMENTS

Importance of the topic

Millions of consumers rely on dietary supplements to support health and well-being, often believing them to be safe and natural. However, the undisclosed presence of pharmaceutical agents poses serious safety risks, especially for products addressing sensitive conditions like sexual dysfunction or weight loss.

Objectives and study overview

This study assessed an open ambient ionisation source (DART) coupled to a portable ACQUITY QDa mass detector for rapid, preparation-free screening of online-purchased herbal supplements. Six products claiming 100% herbal formulations were analysed to detect undeclared active ingredients.

Methodology and instrumentation

The system consisted of a Waters ACQUITY QDa single-quadrupole detector integrated with an IonSense DART ion source using helium at 1.5 mL/min. Both positive and negative ion modes were employed. Temperature and cone voltage ramping facilitated in-source fragmentation, enhancing specificity. Samples were introduced via a ten-sample tablet holder or QuickStrip™ cards without chemical extraction.

Main results and discussion

Undeclared pharmaceuticals were detected in all tested supplements. “Green Devils” capsules contained sildenafil, “Nuvitra” capsules showed sibutramine and fluoxetine, slimming aids yielded bisacodyl fragments, and joint remedies matched diclofenac or acetaminophen spectra. Spectral comparisons against standards and temperature-ramped fragmentation patterns confirmed compound identities. The single-quad system demonstrated reduced false positives compared to UV or ion mobility detectors.

Benefits and practical applications

The DART QDa approach enables rapid <1 min screening with minimal sample handling for tablets, powders or liquids. It can serve as a frontline tool in quality control laboratories or regulatory settings, leveraging library matching for routine surveillance before high-resolution validation.

Future trends and possibilities

Advances may include integration of automated spectral libraries and machine learning for real-time identification, expansion to high-resolution mass detectors, and deployment in point-of-care or field testing to ensure supplement safety.

Conclusion

The open ambient DART QDa system effectively detected various undeclared pharmacologically active compounds in online supplements using a fast, preparation-free workflow. In-source fragmentation and temperature control provided the specificity needed for confident identification.

References

• U.S. Pharmacopeia. www.USP.org
• FDA Consumer Information on Medication Health Fraud. https://www.fda.gov
• Cody RB, Laramee JA, Nilles JM, Durst HD. Direct Analysis in Real Time (DART™), Mass Spectrometry.