1. Liquid Chromatography Tandem Mass Spectrometry and Nuclear Magnetic Resonance Spectroscopy of Magnesium (II) Gluconate Solution
- Author
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Kalyan Kumar Sethi, Snehasis Jana, Parthasarathi Panda, Mahendra Kumar Trivedi, and Trivedi, Mahendra
- Subjects
Electrospray ionization ,Biophysics ,chemistry.chemical_element ,01 natural sciences ,Biochemistry ,High-performance liquid chromatography ,Hypomagnesemia ,03 medical and health sciences ,chemistry.chemical_compound ,0302 clinical medicine ,Liquid chromatography–mass spectrometry ,Magnesium gluconate ,medicine ,030212 general & internal medicine ,Physical and Theoretical Chemistry ,Acetonitrile ,Molecular Biology ,Nuclear magnetic resonance spectroscopy ,Chromatography ,Chemistry ,Magnesium ,010401 analytical chemistry ,medicine.disease ,0104 chemical sciences ,Organometallic ,[SDV.SP] Life Sciences [q-bio]/Pharmaceutical sciences ,Liquid chromatography tandem mass spectrometry ,Gluconic acid - Abstract
Magnesium gluconate is a classical pharmaceutical compound used as a source of magnesium for the prevention and treatment of hypomagnesemia. To the best of our knowledge, a robust and reliable liquid chromatography tandem mass spectrometry technique has not yet been reported for the qualitative and quantitative analysis of magnesium gluconate. This study describes the method development for the LC–ESI–MS/MS analysis of magnesium gluconate using three different reversed-phase HPLC conditions (Method I–III) with comprehensive fragmentation pattern and the structural characterization by NMR spectroscopy. The LC–MS and NMR data were found in accordance with the structure of magnesium gluconate. When magnesium gluconate was dissolved in the acetonitrile and water–methanol solutions, it exists in situ in three different forms: magnesium gluconate itself, gluconic acid, and magnesium gluconate chelate with gluconic acid by a coordinate covalent bond. Method I exhibited pseudo-molecular ion peaks with more magnesium gluconate chelates with gluconic acid, while method II showed an adduct of magnesium gluconate with the solvent along with the molecular ion peak. There was no pseudo-molecular ion peaks found in method III. Thus, method III was found to be the more accurate, robust and reliable LC–MS method for the qualitative and quantitative analysis, structural characterization, and could also be suitable for the pharmacokinetic study of magnesium gluconate. The detailed fragmentation analysis might be useful for the structural characterization of unknown divalent organometallics.
- Published
- 2017