Spectroscopy Solutions for Pharmaceuticals

Significance of the Topic

The reliable performance of UV-Vis spectrophotometers is critical in pharmaceutical research and QA/QC laboratories. Compliance with pharmacopeial standards such as USP <857> ensures accuracy of quantitative assays, supports regulatory audits, and maintains data integrity across the instrument lifecycle.

Objectives and Study Overview

This white paper examines the revisions in USP <857> for operational qualification of UV-Vis spectrophotometers and demonstrates how the Agilent Cary 60 UV-Vis system, paired with Agilent Cary WinUV Validate software, automates and simplifies compliance testing.

Methodology and Instrumentation

The updated USP <857> specifies four performance tests: wavelength control (accuracy and precision), absorbance control (photometric accuracy and precision), stray light, and resolution. Certified reference materials are used for each:

• Holmium perchlorate and didymium CRMs for wavelength accuracy and precision across UV and visible ranges.
• Potassium dichromate solutions and NIST-traceable filters for photometric tests at defined absorbance levels.
• Aqueous salts and acetone solutions to quantify stray light at specified wavelengths.
• Toluene in hexane for spectral resolution assessment between close absorbance peaks.

Instrumentation

The Agilent Cary 60 UV-Vis spectrophotometer features a long-life Xenon flash lamp and no-warmup operation. The WinUV Validate application runs automated test sequences, records replicate measurements, and generates Pass/Fail reports based on user-entered tolerances.

Main Results and Discussion

The Cary 60 meets or exceeds USP <857> criteria:

• Wavelength accuracy within ±1 nm (200–400 nm) and ±2 nm (400–700 nm); precision standard deviation <0.5 nm.
• Photometric accuracy better than ±0.01 Abs below 1 Abs and ±1 % above, with precision limits improved to ±0.005 Abs and ±0.5 % respectively.
• Stray light levels below specified %T thresholds at test wavelengths for chloride, iodide, nitrite, and acetone solutions.
• Spectral resolution ratio consistent with USP requirements for toluene/hexane peaks.

Benefits and Practical Applications

The automated validation workflow reduces manual setup, improves reproducibility, and creates an auditable record to support 21 CFR Part 11 and EU Annex 11 compliance. The Xenon flash lamp reduces maintenance and overall cost of ownership.

Future Trends and Opportunities

Advancements may include integration with LIMS for real-time compliance monitoring, remote diagnostics, predictive maintenance via machine learning, and expanded software capabilities for other pharmacopeial methods.

Conclusion

The Agilent Cary 60 UV-Vis spectrophotometer combined with WinUV Validate software provides a comprehensive solution for meeting updated USP <857> requirements. Automated testing ensures confidence in wavelength and absorbance performance, stray light rejection, and resolution, streamlining QA/QC workflows.

Reference

• Agilent Technologies Support for Title 21 CFR Part 11 and Annex 11 Compliance Agilent Cary WinUV Pharma White Paper 5991-7268EN 2016