Application of capillary electrophoresis-nano-electrospray ionization-mass spectrometry for the determination of N-nitrosodimethylamine in pharmaceuticals

0538745 - ÚIACH 2022 RIV DE eng J - Journal Article
Řemínek, Roman - Foret, František - Chung, D. S.
Application of capillary electrophoresis-nano-electrospray ionization-mass spectrometry for the determination of N-nitrosodimethylamine in pharmaceuticals.
Electrophoresis. Roč. 42, č. 4 (2021), s. 334-341. ISSN 0173-0835. E-ISSN 1522-2683
R&D Projects: GA MŠMT(CZ) 8F17003
Institutional support: RVO:68081715
Keywords : capillary electrophoresis * mass spectrometry * nano-electrospray ionization * N-nitrosodimethylamine
OECD category: Analytical chemistry
Impact factor: 3.595, year: 2021
Method of publishing: Limited access

After a presence of highly hepatotoxic and potentially carcinogenic N-nitrosodimethylamine was detected in certain lots of sartan, ranitidine, metformin, and other pharmaceuticals, local regulatory authorities issued recalls of suspected products, and concerns of the pharmacotherapy safety were widely discussed. Since then, testing of a representative sample of each produced lot of these pharmaceuticals is required as a part of quality control processes. Hence, an interface-free CE-nanoESI system coupled with MS detection was employed for the development of a simple and economical method for quantitative detection of this contaminant in the valsartan drug substances and finished formulations used as model matrices. In this arrangement, a fused-silica capillary was used as both a separation column and a nanoESI emitter providing high ionization efficiency and sensitivity. The optimized procedure was found to have sufficient selectivity, linearity, accuracy, and precision. The established LOD and LOQ values were 0.3 and 1.0 ng/mL, respectively. The practical applicability of the method was tested by analyses of commercially available Valsacor(R) tablets. The results obtained prove that the developed procedure represents a promising alternative to currently available GC- and LC-based methods. Furthermore, after an adjustment of the separation conditions, the CE-nanoESI/MS system can be conceptually used for the determination of NDMA in other suspected pharmaceuticals.
Permanent Link: http://hdl.handle.net/11104/0316481