Fast Analysis of Naproxen Sodium with the Acclaim Trinity P1 Column and Charged Aerosol Detection
The Application Notebook
The characterization of pharmaceutical salts is critical to the drug development process. Active pharmaceutical ingredient (API) salts influence the solubility, stability and hygroscopicity of pharmaceuticals and affect the final drug formulation. Traditionally, the analysis of the API and its counterion salt requires separate applications. Nanopolymer silica hybrid (NSH) technology in the Acclaim Trinity P1 column along with the Corona ultra charged aerosol detector (CAD) enables simultaneous analysis of the API and counterion over four orders of magnitude.
Chris Crafts, Bruce Bailey and Ian Acworth, ESA — A Dionex Company Inc., Chelmsford, Massachusetts, USA.
The characterization of pharmaceutical salts is critical to the drug development process. Active pharmaceutical ingredient (API) salts influence the solubility, stability and hygroscopicity of pharmaceuticals and affect the final drug formulation. Traditionally, the analysis of the API and its counterion salt requires separate applications. Nanopolymer silica hybrid (NSH) technology in the Acclaim Trinity P1 column along with the Corona ultra charged aerosol detector (CAD) enables simultaneous analysis of the API and counterion over four orders of magnitude.
The analysis of a common API (naproxen sodium) with a 3 min isocratic run (Figure 1) is presented here. The range, reproducibility and accuracy of calculation of sodium salts are demonstrated.
Figure 1
Experimental
A standard HPLC system with a Corona ultra sodium acetate and naproxen sodium were from Sigma-Aldrich.
Results
A calibration curve from 5 ng to 10 μg of sodium acetate on column was generated using a quadratic fit function and the x and y axes were inverted (Figure 2), demonstrating the wide dynamic range of the detector. A second curve, from 80 to 300 ng on column (Figure 2 inset), demonstrates the linearity of the detector over small ranges. Both of these curves returned correlation values > 0.99 and reproducibility ≤ 2% for the three injections at each point. The correlation to the theoretical sodium content in the naproxen was then calculated from each curve using a sample of ~800 ng naproxen sodium on column. Recoveries were within 3% of theoretical for the full range curve and within 1% for the linear curve (Table 1).
Figure 2
Conclusion
The CAD response curve towards sodium (as acetate salt) shown in Figure 2 illustrates that an excellent correlation can be calculated even when a wide dynamic range (low nanogram to microgram quantities on column) is used. The accuracy and reproducibility data are sufficient for both research and QC environments. This analytical approach provides accurate and reproducible data for both the API and the counterion salt. As a result of the speed of the method there is an opportunity for significant cost savings during the drug development process. The example can be expanded to other APIs containing both inorganic and/or organic salts.
Table 1: Theoretical and calculated values for sodium.
Acclaim, CAD and Corona are registered trademarks and ultra and Trinity are trademarks of Dionex Corporation.
ESA — A Dionex Company Inc.
22 Alpha Road, Chelmsford, Massachusetts 01824, USA
tel. +1 978 250 7000 fax +1 978 250 7087
Websites: www.esainc.com, www.dionex.com
New Study Uses MSPE with GC–MS to Analyze PFCAs in Water
January 20th 2025Scientists from the China University of Sciences combined magnetic solid-phase extraction (MSPE) with gas chromatography–mass spectrometry (GC–MS) to analyze perfluoro carboxylic acids (PFCAs) in different water environments.
The Next Frontier for Mass Spectrometry: Maximizing Ion Utilization
January 20th 2025In this podcast, Daniel DeBord, CTO of MOBILion Systems, describes a new high resolution mass spectrometry approach that promises to increase speed and sensitivity in omics applications. MOBILion recently introduced the PAMAF mode of operation, which stands for parallel accumulation with mobility aligned fragmentation. It substantially increases the fraction of ion used for mass spectrometry analysis by replacing the functionality of the quadrupole with high resolution ion mobility. Listen to learn more about this exciting new development.
A Guide To Finding the Ideal Syringe and Needle
January 20th 2025Hamilton has produced a series of reference guides to assist science professionals in finding the best-suited products and configurations for their applications. The Syringe and Needle Reference Guide provides detailed information on Hamilton Company’s full portfolio of syringes and needles. Everything from cleaning and preventative maintenance to individual part numbers are available for review. It also includes selection charts to help you choose between syringe terminations like cemented needles and luer tips.
The Complexity of Oligonucleotide Separations
January 9th 2025Peter Pellegrinelli, Applications Specialist at Advanced Materials Technology (AMT) explains the complexity of oligonucleotide separations due to the unique chemical properties of these molecules. Issues such as varying length, sequence complexity, and hydrophilic-hydrophobic characteristics make efficient separations difficult. Separation scientists are addressing these challenges by modifying mobile phase compositions, using varying ion-pairing reagents, and exploring alternative separation modes like HILIC and ion-exchange chromatography. Due to these complexities, AMT has introduced the HALO® OLIGO column, which offers high-resolution, fast separations through its innovative Fused-Core® technology and high pH stability. Alongside explaining the new column, Peter looks to the future of these separations and what is next to come.
Oasis or Sand Dune? Isolation of Psychedelic Compounds
January 20th 2025Magic mushrooms, once taboo, have recently experienced a renaissance. This new awakening is partially due to new findings that indicate the effects of psilocybin, and its dephosphorylated cousin psilocin may produce long lasting results for patients who might be struggling with anxiety, depression, alcohol and drug abuse, and post-traumatic stress disorder. Hamilton Company has developed a methodology for the isolation and identification of 5 common psychedelic compounds used in the potential treatment of disease. The PRP-1 HPLC column resin remains stable in the harsh alkaline conditions ideal for better separations.
