Agilent OpenLab CDS for Automated High Throughput Purity Assessment Using Mass Spectrometry

Significance of the Topic

Purity assessment of chemical samples is a critical step across organic synthesis, pharmaceutical development, formulation optimization, and QA/QC laboratories. Accurate determination of sample purity ensures reliable yield estimates, confirms compound identity before biological testing, supports formulation stability studies, and validates that intermediates and final products meet regulatory quality standards. High-throughput methods with minimal manual interpretation empower bench chemists to make rapid decisions without relying on central analytical services.

Objectives and Study Overview

This application note describes how Agilent OpenLab CDS software, in combination with an InfinityLab LC/MSD XT system, automates compound confirmation and purity determination workflows. Using a simulated degradation experiment, six pharmaceutical standards stored under refrigeration for four months were analyzed by LC/MS. The goal was to demonstrate a fully automated process—from data acquisition to reporting—that identifies target compounds, calculates purity levels, and highlights degraded samples within a batch.

Methodology and Applied Instrumentation

Standards of Buspirone, Amitriptyline, Nefazodone, Clopidogrel, Paclitaxel, and Fosinopril were prepared at 1 mg/mL in acetonitrile, stored for four months, then diluted to 20 ng/μL in 20% ACN. A 4-minute generic LC method on a 2.1 × 50 mm Poroshell 120 EC-C18 column employed water/ACN with 0.1% formic acid. The Agilent InfinityLab single-quadrupole LC/MSD XT, equipped with an ESI source and Jet Stream technology, acquired full-scan data (100–900 m/z) at 2 scans/s in positive mode. OpenLab CDS v2.2 managed sequence setup, target mass entry, automated processing, and report generation.

Main Results and Discussion

Compound confirmation relied on extracted ion chromatograms (EICs) for [M+H]+ (and potential adducts) overlapping with total ion chromatogram (TIC) peaks. Purity was calculated by comparing the sum of target-ion peak areas to total signal. For example, Paclitaxel’s EIC area of 950,000 counts versus 1,000,000 total counts yielded 95% purity by TIC. A predefined 80% cutoff was applied across the batch.
OpenLab CDS produced color-coded batch summaries identifying four compounds above the cutoff and two below. Detailed review of individual samples provided EIC/TIC/UV traces and mass spectra for impurity characterization. Automated report templates delivered clear, colored indications of compound presence and pass/fail purity status.

Benefits and Practical Applications

• Enables bench-level purity testing without expert MS interpretation.
• Reduces laboratory footprint by stacking MSD with LC modules.
• Streamlines workflow through automated data processing and color-coded reporting.
• Allows rapid reprocessing by updating target masses without reinjection.

Future Trends and Potential Uses

Emerging applications may integrate additional universal detectors (e.g., ELSD) in series with MS for multi-detector purity assessment. Advanced data analytics and machine learning could enhance impurity profiling and automate method optimization. Further miniaturization and cloud-based data sharing promise even higher throughput and remote collaboration for real-time decision-making.

Conclusion

The combination of Agilent OpenLab CDS and InfinityLab LC/MSD XT delivers a robust, fully automated solution for high-throughput sample purity assessment. By minimizing manual interpretation and leveraging color-coded reports, this workflow empowers chemists to confirm compound identity and purity quickly and reliably, improving laboratory productivity and decision-making efficiency.