Multicomponent Analysis of Fat- and Water-Soluble Vitamins and Auxiliary Substances in Multivitamin Preparations by qNMR

Abstract

A nuclear magnetic resonance (NMR) spectroscopic method was tested to control 12 vitamins and accompanying substances in multivitamin preparations. The limits of detection (LODs) and limits of quantification (LOQs) varied in the 9.0-77.0 mg/kg and in the 34.5-93.5 mg/kg range, respectively. The coefficients of variation (CVs) ranged between 0.9% and 12%. The (1)H NMR spectra showed linearity for the 140-260 mg sample weight (R(2) > 0.918). The NMR spectra of multivitamin preparations showed the presence of different degradation products of ascorbic acid. The NMR method was applied to 13 different multivitamin preparations including tablets, capsules, and effervescent tablets with average recovery rates between 85% and 132%. A number of accompanying substances (citric acid, mannitol, saccharin, cyclamate, sum of steviol glycosides, and butylhydroxytoluene) were additionally identified and quantified. NMR was found to be suitable for the simultaneous qualitative measurement of water- and fat-soluble vitamins and accompanying substances and shows some promise for quantitative determination of at least 5 vitamins (B1, B3, B5, B6, and E) in multivitamin preparations.

Facilitating the performance of qNMR analysis using automated quantification and results verification

“…Nowadays quantitative nuclear magnetic resonance (qNMR) is a well‐established procedure to estimate the concentrations of multiple compounds in complex mixtures . The main application areas of qNMR are drug discovery, food and beverage control and clinical diagnostics . Moreover, several qNMR studies deal with determining purity of organic molecules .…”

Monitoring daily routine performance in quantitative NMR (qNMR) spectroscopy: Is the system suitability test necessary?

“…Nuclear magnetic resonance (NMR) technology has been dramatically improved in the last decades and is now considered as a premiere analytical method for quantitative (q) analysis of complex mixtures . As a consequence, along with the worldwide recognition and propagation of this technique, the number of daily NMR experiments is constantly increasing.…”

“…Nuclear magnetic resonance (NMR) technology has been dramatically improved in the last decades and is now considered as a premiere analytical method for quantitative (q) analysis of complex mixtures. [1][2][3][4][5][6][7][8][9][10][11] As a consequence, along with the worldwide recognition and propagation of this technique, the number of daily NMR experiments is constantly increasing. To extract robust information from these data, it is necessary to have a clear and robust standard operation procedure for each step from sample preparation to spectra evaluation.…”

Detection and quantification of vitamins in microliter volumes of biological samples by LC‐MS for clinical screening

“…There are also methods for simultaneous extraction of water‐soluble and fat‐soluble vitamins except they eventually used separate analytical methods for analysis . Although simultaneous detection of water‐soluble and fat‐soluble vitamins in a single chromatography run from a single aliquot of sample has been reported, these methods are only reported to determine vitamin contents in uncomplicated, non‐biological matrices, such as pharmaceutical preparations, foodstuff, and beverages . The method by Ferreiro‐Vera et al was able to determine only two vitamins with different polarities in the blood serum while unified supercritical fluid and liquid chromatography method by Taguchi et al was only validated with standard solutions.…”