Structural studies of pharmaceutical products using the ARL EQUINOX 100 X-ray benchtop Diffractometer

Importance of Topic

X-ray diffraction (XRD) is a cornerstone technique in pharmaceutical analysis for characterizing solid forms, crystallinity and polymorphism of active pharmaceutical ingredients (APIs). It plays a central role from early drug discovery through formulation development, stability testing and quality control. Fast, reliable XRD data assists in ensuring product performance, bioavailability and regulatory compliance.

Objectives and Study Overview

This application note presents the capabilities of the Thermo Scientific ARL EQUINOX 100 benchtop XRD system for structural analysis of pharmaceutical products. Key goals include demonstrating rapid data acquisition, evaluation of polymorphs and salts, assessment of crystallinity and the system’s adaptability for routine QA/QC and research tasks.

Methodology and Instrumentation

The ARL EQUINOX 100 employs a 60 W microfocus X-ray source (Cu or Co) with a curved position sensitive detector (CPS) covering the full 2θ range (1–110°) in real time. No external chillers are required, allowing portable operation. Both reflection and transmission modes are supported on the same platform. Optional stages include controlled‐atmosphere cells, spinning sample holders, capillaries and automated sample changers. Data acquisition and processing are managed through integrated software compliant with 21 CFR Part 11 for secure electronic records.

Main Results and Discussion

• Real-time acquisition of diffraction patterns enables dynamic monitoring of crystallization processes.
• Reflection and transmission measurements on paracetamol tablets achieved full scans from 2° to 100° 2θ in minutes, illustrating high throughput.
• Comparison of analysis modes showed consistent phase identification and peak resolution suitable for polymorph screening.
• Fast data collection reduces sample exposure time and accelerates decision-making in development pipelines.

Benefits and Practical Applications

• Efficient polymorph, salt and co‐crystal screening in preformulation studies
• Quantitative crystallinity determination for batch release and stability testing
• Flexible sample environments for studying reactivity under controlled temperature and atmosphere
• Routine QA/QC operations with minimal lab infrastructure requirements

Future Trends and Opportunities

Advances may include integration of automated high-throughput workflows, in situ reaction monitoring under varied conditions and coupling with complementary techniques (e.g. Raman, DSC). Implementation of artificial intelligence for pattern recognition and predictive analysis could further streamline polymorph identification and quality assessment.

Conclusion

The ARL EQUINOX 100 benchtop XRD system offers rapid, high‐quality diffraction data with flexible sample handling and compliance features ideal for pharmaceutical research and routine quality control. Its compact design and real-time full‐range CPS detector support accelerated workflows from early screening to stability studies, enhancing analytical capabilities in modern laboratories.