Journal
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
Volume 413, Issue 6, Pages 1701-1714Publisher
SPRINGER HEIDELBERG
DOI: 10.1007/s00216-020-03134-1
Keywords
Purity; Metrological traceability; Quantitative nuclear magnetic resonance; Nitrofuran metabolites
Funding
- Carlos Chagas Filho Research Support Foundation of the Rio de Janeiro State FAPERJ [E-26/110.135/2013]
- National Council for Scientific and Technological Development (CNPq)
- FAPERJ [303086/2015-7, E-26/202.834/2017]
Ask authors/readers for more resources
The comparability and metrological traceability of measurement results are crucial for reliable decision-making. Using certified reference materials and potential primary reference measurement procedures are necessary in analytical chemistry to ensure traceable measurements. In this work, qNMR was used to determine the purity of nitrofuran metabolites with consistent results compared to those obtained by mass balance approach.
Comparability of measurement results and their metrological traceability to the International System of Units (SI) are fundamental tools to ensure reliable decisions in the social sphere, commerce, and science. The use of appropriate references in analytical chemistry, such as certified reference materials (CRMs) of high purity substances, is one of the required procedures to obtain traceable measurements. When commercial standards with non-certified purity values are used, traceability must be achieved by determining the purity of the standard using a potential primary reference measurement procedure or other appropriate methods. Quantitative nuclear magnetic resonance (qNMR) is a technique with the potential to be used in primary measurement procedures. This work presents the determination of purity by H-1 qNMR for nitrofuran metabolites 3-amino-2-oxazolidinone (AOZ), 3-amino-5-morpholinomethyl-2-oxazolidinone (AMOZ), and 1-aminohydantoin (AHD). Furthermore, a recent qNMR method developed by our group to improve the quantitative performance of measurements using C-13 nucleus was used to determine the purity of semicarbazide (SEM) nitrofuran metabolite. Purity values obtained by qNMR for AOZ, AMOZ, and AHD standards were compared to values obtained by the mass balance approach using a suite of analytical methods: Karl Fischer (KF) coulometric titration and thermogravimetry (TG) for the determination of water and residual solvents, gas and liquid chromatography for the determination of impurities structurally related to the metabolites. The results obtained by qNMR and mass balance were consistent.
Authors
I am an author on this paper
Click your name to claim this paper and add it to your profile.
Reviews
Recommended
No Data Available