Quantitative proton magnetic resonance determination of N,N-dimethylformamide in one intermediate of the Quimi-Hib vaccine.
Quimi-Hib is a conjugate vaccine against Haemophilus influenza type b (Hib) where the Hib antigen is the only one produced by chemical synthesis. NMR has become the alternative of choice for the identity of intermediates during the chemical synthesis of Hib antigen. We explore a rapid quantitative proton magnetic resonance (qHNMR) assay for the determination of N,N-dimethylformamide (DMF) as a residual in one of the critical intermediates. The proposed assay has been shown to be accurate, precise for intermediate precision conditions (relative standard deviation <3% for spectrometer-to-spectrometer variations), specific (no detected interferences), and rugged (percentage difference <3% for day-to-day and spectrometer-to-spectrometer variations). The quantitative NMR assay can replace the common chromatographic methods for monitoring the DMF contents in one crucial step of the synthetic scheme.
Center of Biomolecular Chemistry, 200 Street and 21 Ave. Atabey, Playa, La Habana, Cuba 11600. raine.garrido@cqb.cu
Raine
R
Garrido Arteaga
Felix
F
Cardoso San Jorge
María del C
Mdel C
Rodríguez Montero
Violeta
V
Fernández Santana
Vicente
V
Vérez Bencomo
Herman
H
Vélez Castro
D004126:Dimethylformamide / Q000032:analysis*; D018073:Haemophilus Vaccines / Q000737:chemistry*; D009682:Magnetic Resonance Spectroscopy; D008968:Molecular Conformation; D011522:Protons; D018074:Vaccines, Conjugate / Q000737:chemistry
D018073:Haemophilus Vaccines; D011522:Protons; D018074:Vaccines, Conjugate; D004126:Dimethylformamide