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

Dietary supplements are widely consumed for health and wellness benefits, but undeclared pharmaceutical ingredients pose serious safety risks. Rapid, preparation-free screening methods are essential to detect harmful adulterants, protect consumers, and support regulatory enforcement.

Objectives and Overview of the Study

This work evaluates the performance of an open ambient ionisation source coupled to a portable single-quadrupole mass detector (DART QDa System) as a tool for fast, on-site detection of undeclared active pharmaceutical ingredients in online-purchased health supplements.

Methodology and Instrumentation

The study employed helium-based DART ionisation in positive and negative modes, utilising in-source fragmentation and adjustable gas temperatures (150 °C–450 °C) and cone voltages (5 V–100 V) for enhanced compound specificity.

• Sample introduction methods: single tablet holder in a 45° DART gun fixture and 12-position QuickStrip cards.
• Analysis parameters: fixed helium flow (1.5 mL/min) and systematic temperature and voltage ramps.

Instrumentation Used

• Waters ACQUITY QDa Mass Detector
• IonSense DART® Ion Source

Main Results and Discussion

Multiple undeclared actives were identified across supplement categories:

• Male potency aids contained sildenafil and tadalafil.
• Slimming products revealed sibutramine, fluoxetine and bisacodyl.
• Joint remedies showed NSAIDs such as diclofenac and acetaminophen.

Comparison with analytical standards under identical conditions confirmed compound identities. Temperature-dependent ionisation and in-source fragmentation improved spectral confidence and reduced false positives compared to traditional UV or mobility-based detectors.

Benefits and Practical Applications of the Method

• Rapid, sample-prep-free analysis (< seconds per sample)
• Applicable to various forms (tablets, powders, natural products)
• Portable setup suitable for field screening by regulatory agencies and quality control laboratories

Future Trends and Potential Applications

Integration with spectral library matching and profile-matching software could automate result interpretation. Coupling with high-resolution MS would enable full confirmation of unknowns. The approach may extend to screening for illicit drugs, mycotoxins, pesticides and environmental contaminants.

Conclusion

The DART QDa System provides a robust, first-line screening platform for rapid detection of undeclared pharmaceuticals in dietary supplements. Its minimal sample preparation, speed, and specificity make it a valuable tool for consumer safety and regulatory compliance.

References

1. Waters Corporation. Direct Analysis in Real Time (DART™) Mass Spectrometry. Robert B. Cody et al.
2. U.S. Pharmacopeia. www.usp.org.
3. U.S. Food and Drug Administration. Medication Health Fraud. fda.gov.
4. Cody RB, Laramee JA, Nilles JM, Durst HD. Direct Analysis in Real Time (DART™). Anal. Chem.