Stability-indicating proton nuclear magnetic resonance spectroscopic method for determination of S-adenosyl-L-methionine in tablets.

L. K. Revelle, D. A. d'Avignon, J. C. Reepmeyer, R. C. Zerfing

Research output: Contribution to journalArticle

13 Scopus citations

Abstract

We present a simple, accurate, stability-indicating nuclear magnetic resonance (NMR) method for determining active (S,S) and inactive (R,S) epimers of S-adenosyl-L-methionine (SAM) in tablets. The SCH3 resonances of SAM epimers were well resolved at 300 MHz. Individual assays of 5 SAM tablets gave SAM values of 101.3 +/- 1.7% of declared amounts. Tablet solutions were assayed at a level of 8.0 mg/mL, but the method was linear for SAM concentrations ranging from 64 to 1 mg/mL (correlation coefficient, 0.9996). Reproducibility was indicated by a relative standard deviation of 0.33% for 6 replicate assays for total SAM at a concentration of 8 mg/mL. In contrast to the propietary liquid chromatographic (LC) method, which requires SAM as an external standard, the NMR method uses sodium trimethylsilylpropionate-d4 (TSP) both as an internal standard and as a chemical shift reference. The method was used to test the stability of SAM analytes under various pH levels and temperatures. We found 8% inactivation of SAM due to epimerization over a 24 h period at room temperature and pH 5. SAM solutions showed no detectable inactivation after 14 days when stored below 0 degrees C.

Original languageEnglish (US)
Pages (from-to)353-358
Number of pages6
JournalJournal of AOAC International
Volume78
Issue number2
DOIs
StatePublished - Jan 1 1995
Externally publishedYes

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