Analysis of Pharmaceutical Products

Significance of the Topic

Elemental analysis of pharmaceutical tablets is a critical component of quality control and regulatory compliance in the drug manufacturing industry. By accurately identifying and quantifying both active pharmaceutical ingredients and excipient elements, laboratories can ensure product safety, efficacy and batch consistency. Energy‐dispersive X‐ray fluorescence (EDX) offers a rapid, non‐destructive approach that minimizes sample preparation and supports high‐throughput testing.

Objectives and Study Overview

This application note evaluates the performance of the Shimadzu EDX‐700/800 series for the analysis of a cold tablet formulation. Key goals include:

• Determining which elements can be detected and quantified without chemical standards
• Assessing the repeatability of quantitative measurements across multiple runs

Methodology and Instrumentation

A single, intact tablet was placed directly on a standard sample holder with no further preparation. Measurements were performed under vacuum using the following conditions:

• Instrument: Shimadzu EDX‐800
• X‐ray tube: Rhodium anode, 15–50 kV at 15–200 µA
• Dead time: 25 %
• Beam diameter: 10 mm
• Acquisition time: 100 s
• No filter applied

The system employed a fundamental‐parameter (FP) model for standardless quantification. Spectra were acquired to cover light elements (Na through Ca) and heavier halogens (Br).

Main Results and Discussion

Quantitative analysis revealed the following composition by weight percentage:

• Silicon (Si): 0.98 %
• Chlorine (Cl): 0.46 %
• Sodium (Na): 0.12 %
• Bromine (Br): 0.10 %
• Sulfur (S): 0.079 %
• Magnesium (Mg): 0.035 %
• Phosphorus (P): 0.026 %
• Calcium (Ca): 0.011 %
• Active compound (C8H9NO2): 98.19 %

Precision was evaluated over repeated measurements of Cl and Br:

• Chlorine: mean 0.464 %, SD 0.0070 %, CV 1.5 %
• Bromine: mean 0.103 %, SD 0.00063 %, CV 0.61 %

These results demonstrate excellent repeatability and low relative uncertainty for both light and mid‐Z elements using the EDX‐800.

Benefits and Practical Applications

The method offers several advantages for pharmaceutical quality assurance:

• No chemical reagents or complex sample prep required
• Rapid turnaround time (measurement in under two minutes)
• Non‐destructive testing preserves the original sample
• Standardless quantification simplifies workflow and reduces calibration needs

This approach can be integrated into routine batch testing, impurity screening and stability studies.

Future Trends and Potential Uses

Emerging developments may further enhance EDX applications in pharma:

• Automated sample handling and robotics for higher throughput
• Advanced spectral deconvolution algorithms using machine learning
• Portable EDX instruments for on‐site testing in manufacturing plants
• Extension to trace‐level impurities and heavy metal screening

Conclusion

The Shimadzu EDX‐700/800 platform delivers reliable, precise elemental analysis of pharmaceutical tablets without sample preparation. Its speed, ease of use and solid repeatability make it a valuable tool for quality control and research laboratories in the pharmaceutical industry.