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Quantitative 1H NMR method for analyzing primaquine diphosphate in active pharmaceutical ingredients
Rafaella C de A Silva1, Eduardo G R de Sousa1, José Luiz Mazzei1
1Fundação Oswaldo Cruz, Farmanguinhos, Rua Sizenando Nabuco, 100, Manguinhos, 21041-250 Rio de Janeiro, RJ, Brazil.
Journal of Pharmaceutical and Biomedical Analysis
|January 18, 2022
Summary
This study elucidates primaquine diphosphate (PQD) structures using advanced NMR techniques for malaria medicine quality control. A validated quantitative NMR (qNMR) method was developed for accurate PQD content determination in active pharmaceutical ingredients.
Area of Science:
- Analytical Chemistry
- Pharmaceutical Analysis
- Spectroscopy
Background:
- Primaquine diphosphate (PQD) is crucial for malaria treatment, necessitating robust quality control measures.
- Accurate quantification of PQD in active pharmaceutical ingredients (APIs) is essential for ensuring drug efficacy and patient safety.
- Existing analytical methods may require enhancement for speed, specificity, and reliability in PQD analysis.
Purpose of the Study:
- To fully characterize and elucidate the structures of primaquine diphosphate (PQD) samples.
- To develop and validate a simple, rapid, specific, and reliable quantitative NMR (qNMR) method for determining PQD levels in APIs.
- To support and endorse current pharmacopoeial methods for PQD content determination.
Main Methods:
- Comprehensive structural elucidation using thermal analysis, Fourier Transform IR, and various solution and solid-state NMR techniques (1D, 2D, 13C, 31P MAS NMR).
- Development of a quantitative NMR (qNMR) method utilizing ethylene carbonate (EC) as an internal standard in DMSO-d6.
- Validation of the qNMR method according to international guidelines, assessing linearity, range, LOD/LOQ, stability, precision, robustness, and accuracy.
Main Results:
- Detailed structural information of PQD samples was obtained through extensive spectroscopic analysis.
- A validated qNMR method was established for the precise quantification of PQD in APIs, using specific 1H NMR signals.
- The qNMR method demonstrated excellent performance, with accuracy comparable to pharmacopeial HPLC techniques (p > 0.05).
Conclusions:
- The employed NMR techniques provide comprehensive structural insights into PQD.
- The developed qNMR method offers a reliable and efficient alternative for PQD quantification in pharmaceutical quality control.
- This qNMR approach complements and validates existing pharmacopoeial methods, enhancing API analysis capabilities.
