Analysis of Fenoprofen Using a Core Enhanced Technology Accucore HPLC Column

Significance of the Topic

Fenoprofen is a widely used nonsteroidal anti-inflammatory drug (NSAID) prescribed for pain, fever, and inflammation management in rheumatic and joint disorders. Rapid and reliable chromatographic analysis of fenoprofen is essential for quality control in pharmaceutical production and regulatory compliance according to pharmacopeial standards.

Objectives and Study Overview

This study aimed to adapt the United States Pharmacopeia (USP) monograph method for fenoprofen analysis to a smaller, high-efficiency superficially porous HPLC column. By applying an in-house method transfer calculator, the USP procedure was scaled down to reduce runtime and solvent consumption while maintaining or improving performance criteria.

Methodology

A mixed standard solution containing fenoprofen and internal standard gemfibrozil was prepared at 100 µg/mL in 50:50 methanol:water. Chromatographic separation was achieved under the following conditions:

• Mobile phase: 50:49.6:0.4 acetonitrile:water:phosphoric acid
• Column temperature: 30 °C
• Flow rate: 0.4 mL/min
• Injection volume: 3 µL
• Detection wavelength: 272 nm

Instrumental Setup

Key equipment and consumables included:

• Accucore RP-MS superficially porous column, 2.6 µm, 100 × 2.1 mm
• Thermo Scientific HPLC system capable of 200 bar backpressure
• HPLC-grade solvents: acetonitrile and water
• Phosphoric acid additive
• NSC Mass Spec certified vials with bonded PTFE/silicone caps

Main Results and Discussion

Using the scaled-down method, fenoprofen eluted at 1.63 min (tailing factor 1.23) and gemfibrozil at 3.67 min (tailing factor 1.22). Resolution between the peaks exceeded 14, surpassing the USP requirement of >8. Method precision, expressed as %RSD over six injections, was below 0.5% for retention time and peak shape metrics, demonstrating robust performance.

The superficially porous particle design provided high efficiency, low peak tailing, and reduced backpressure relative to traditional sub-2 µm fully porous columns. The shorter run time (<2 min for analyte) supports high sample throughput and lower solvent usage.

Benefits and Practical Applications

This optimized HPLC method offers several advantages for pharmaceutical quality control laboratories:

• Significantly reduced analysis time, enabling more samples per day
• Lower solvent consumption and operating costs
• Compliance with USP criteria for fenoprofen assay
• Compatibility with existing HPLC platforms operating at moderate pressure

Future Trends and Applications

Further developments may include coupling superficially porous columns with mass spectrometric detection for enhanced specificity, integration into automated high-throughput workflows, and continued miniaturization towards microflow applications. Green analytical chemistry approaches may drive even lower solvent usage and waste generation.

Conclusion

The application of a Core Enhanced Technology Accucore RP-MS column enables rapid, robust, and USP-compliant analysis of fenoprofen. The scaled-down method significantly improves sample throughput and cost efficiency, making it a valuable tool for pharmaceutical quality control.

References

1. Thermo Fisher Scientific. HPLC Method Transfer Calculator.
2. U.S. Food and Drug Administration. Approval documentation for fenoprofen.
3. United States Pharmacopeia. Monograph for Fenoprofen.