XRD Investigation of Ibuprofen with ARL EQUINOX 100 in Transmission Mode

Importance of the topic

Powder X-ray diffraction (XRD) is a versatile and sensitive analytical method widely used in pharmaceutical research and production to characterize crystalline structures of active pharmaceutical ingredients (APIs) and excipients. It enables rapid phase identification, detection of polymorphs, salts, co-crystals and impurities, as well as monitoring dynamic processes such as crystallization under various conditions, contributing to quality control and formulation development.

Objectives and study overview

• Evaluate the performance of the Thermo Scientific ARL EQUINOX 100 diffractometer in transmission mode for qualitative phase analysis of ibuprofen formulations.
• Compare four commercial ibuprofen products, including brand-name and generic formulations, to identify API and excipient crystalline phases.
• Demonstrate the instrument’s speed and sensitivity for routine pharmaceutical screening.

Methodology and instrumentation

• Sample preparation: Four ibuprofen products from different vendors were finely ground and loaded into transmission cups using adhesive tape.
• Data acquisition: Each sample was rotated and measured for 10 minutes using Cu Kα radiation (λ=1.541874 Å).
• Data processing: Diffraction patterns were analyzed qualitatively using MATCH! software with the Crystallography Open Database (COD).

Main results and discussion

• All brand-name products displayed characteristic ibuprofen peaks alongside distinctive excipient phases such as talc (lubricant), calcium carbonate, sodium citrate and sucrose, with variations reflecting different formulations.
• One generic product exhibited only the ibuprofen crystalline phase, indicating minimal excipient crystallinity.
• The ARL EQUINOX 100’s curved position sensitive detector captured complete diffraction profiles simultaneously, enabling clear resolution of major and trace phases within a 10-minute scan.

Benefits and practical applications

The ARL EQUINOX 100 provides rapid, high-resolution phase analysis without complex alignment or cooling infrastructure, making it ideal for preformulation screening, impurity tracking during synthesis, and quality assurance/quality control (QA/QC) workflows. Its portability allows deployment across multiple laboratories or in-field investigations.

Future trends and applications

• Integration of in situ and non-ambient measurements to monitor real-time crystallization and polymorphic transitions.
• Development of automated workflows and advanced software for quantitative phase analysis and structure determination from powder data.
• Expansion of mobile diffractometer use for on-site quality control and rapid decision making in pharmaceutical manufacturing.

Conclusion

The ARL EQUINOX 100 in transmission mode offers a user-friendly, high-throughput XRD solution for pharmaceutical research and production, delivering clear phase identification of ibuprofen formulations and excipients within minutes. Its sensitivity to trace components and minimal infrastructure requirements position it as a valuable tool from preformulation to final product QA/QC.

References

• Thermo Fisher Scientific. Application Note AN41106: XRD Investigation of Ibuprofen with ARL EQUINOX 100 in Transmission Mode. 2017.