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Published on: August 9, 2022
Improved solid-state NMR quantifications of active principles in pharmaceutical formulations.
Stéphanie Sanchez1, Fabio Ziarelli, Stéphane Viel
1Aix-Marseille Université, ISM2-UMR-6263, Equipe CES, case 512, av. Escadrille Normandie Niémen, 13397 Marseille Cedex 20, France.
Solid-state nuclear magnetic resonance (ssNMR) enables rapid and precise quantification of active pharmaceutical ingredients in solid formulations. This method simplifies analysis by eliminating the need for sample solubilization, offering an efficient alternative for pharmaceutical quality control.
Area of Science:
- Pharmaceutical Sciences
- Analytical Chemistry
- Materials Science
Background:
- Solid-state nuclear magnetic resonance (ssNMR) spectroscopy is increasingly utilized in pharmaceutical analysis.
- Approximately 80% of pharmaceutical formulations are solid-based, necessitating efficient analytical methods.
- Traditional methods may require sample solubilization, adding complexity and time.
Purpose of the Study:
- To develop a fast and precise method for quantifying active pharmaceutical ingredients in solid formulations using ssNMR.
- To optimize sample preparation and referencing for accurate quantitative ssNMR analysis.
- To demonstrate the method's efficacy using a commercial pharmaceutical product.
Main Methods:
- Utilized solid-state MAS NMR spectroscopy for analysis.
- Implemented external concentration referencing.
- Developed optimized sample preparation protocols for quantitative ssNMR.
- Applied the method to quantify Meprobamate in a commercial formulation (Equanil).
Main Results:
- Achieved fast and precise quantification of active principles in solid pharmaceutical formulations.
- Demonstrated the effectiveness of combining external referencing and optimized sample preparation.
- Successfully reinvestigated the dosage of Meprobamate in Equanil with high accuracy.
- The developed ssNMR protocol offers significant advantages over previously proposed analytical methods.
Conclusions:
- ssNMR spectroscopy, with appropriate methodology, provides a rapid and precise tool for pharmaceutical formulation analysis.
- The optimized protocol overcomes limitations of traditional methods, enhancing efficiency in drug quantification.
- This approach is highly valuable for quality control and development in the pharmaceutical industry.
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