Abstract
Solid-state 13C NMR spectra of tablets or capsules of prednisolone, enalapril maleate, lovastatin, simvastatin, ibuprofen, flurbiprofen, mefenamic acid, indomethacin, diflunisal, sulindac, and piroxicam were obtained in the CP/MAS mode at 50 MHz. These studies show that (1) solid-state NMR spectroscopy can detect the active ingredients in low-dose tablets and capsules; (2) the use of interrupted decoupling often results in suppression of resonances due to excipients, thereby allowing better detection of resonances from the drug; and (3) the technique permits discrimination between two prednisolone polymorphs present in tablets obtained from various manufacturers even though the tablets contain only approximately 5% (w/w) of the drug.
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REFERENCES
J. Schaefer and E. O. Stejskal. Carbon-13 nuclear magnetic resonance of polymers spinning at the magic angle. J. Am. Chem. Soc. 98:1031–1032 (1976).
S. R. Byrn, G. Gray, R. R. Pfeiffer, and J. Frye. Analysis of solid-state carbon-13 NMR spectra of polymorphs (benoxaprofen and nabilone) and pseudomorphs (cefazolin). J. Pharm. Sci. 74(5):565–568 (1985).
S. R. Byrn, P. A. Sutton, and B. Tobias. The crystal structure, solid-state NMR spectra and oxygen reactivity of five crystal forms of prednisolone tert-butylacetate. J. Am. Chem. Soc. 110:1609–1614 (1988).
D. P. Ip, G. S. Brenner, J. M. Stevenson, S. Lindenbaum, A. W. Douglas, S. D. Klein, and J. A. McCauley. High resolution spectroscopic evidence and solution calorimetry studies on the polymorphs of enalapril maleate. Int. J. Pharm. 28:183–191 (1986).
R. Suryanaryanan and T. S. Wiedmann. Quantitation of the relative amounts of anhydrous carbamazepine and carbamazepine dihydrate in a mixture by solid-state nuclear magnetic resonance. Pharm. Res. 7:184–187 (1990).
C.-j. Chang, L. E. Diaz, F. Morin, and D. Grant. Solid-state carbon-13 NMR study of drugs: Aspirin. Magnet. Res. Chem. 24:768 (1986).
L. E. Diaz, L. Frydman, A. Olivieri, and B. Frydman. Solidstate NMR of drugs: Soluble aspirin. Anal. Lett. 20:1657 (1987).
N. R. Jagannathan. High resolution solid-state carbon-13 nuclear magnetic resonance study of acetaminophen. Curr. Sci. 56(16):827–830 (1987).
J. P. Hickey, I. S. Butler, and G. Pouskouleli. Carbon-13 NMR spectra of some representative hormonal steroids. J. Magnet. Res. 38:501 (1980).
R. N. Moore, G. Bigam, J. K. Chan, A. M. Hogg, T. T. Nakashima, and J. C. Vederas. Biosynthesis of the hypocholesterolemic agent mevinolin by Aspergillus terreus. Determination of the origin of carbon, hydrogen, and oxygen atoms by 13C NMR and mass spectrometry. J. Am. Chem. Soc. 107:3694–3701 (1985).
S. J. Opella, M. H. Frey, and T. A. Cross. Selection of non-protonated carbon resonances in solid-state nuclear magnetic resonance. J. Am. Chem. Soc. 101:5854–5857 (1979).
Y.-G. Smeyers, S. Cuellare-Rodriguez, E. Galvez-Ruano, and M. S. Arias-Perez. Conformational analysis of some α-phenylpropronic acids with anti-inflammatory activity. J. Pharm. Sci. 74:47–49 (1985).
Y.-G. Smeyers, A. Hernandez-Laguna, C. Munoz-Caro, J. Aguilera, E. Galvez-Ruano, and M. S. Arias-Perez. Quantum mechanical study: Nuclear magnetic resonance measurements of some α-arylcarboxy alkyl acids as anti-inflammatory agents. J. Pharm. Sci. 78:764–766 (1989).
M. O'Brien, J. McCauley, E. Cohen, and K. Florey (eds.). Analytical Profiles of Drug Substances, Vol. 13, Academic Press, New York, 1984, pp. 211–238.
M. L. Cotton, R. A. Hux, and K. Florey (ed.). Analytical Profiles of Drug Substances, Vol. 14, Academic Press, New York, 1985, pp. 491–526.
A. W. Douglas. Carbon-13 nuclear magnetic resonance studies of (Z)-5-fluoro-Z-methyl-1-{[p-(methylsulfinyl)phenyl]methylene}-1H-indene-3-acetic acid (sulindac) and some related compounds. Can. J. Chem. 56:2129–2133 (1978).
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Saindon, P.J., Cauchon, N.S., Sutton, P.A. et al. Solid-State Nuclear Magnetic Resonance (NMR) Spectra of Pharmaceutical Dosage Forms. Pharm Res 10, 197–203 (1993). https://doi.org/10.1023/A:1018922407786
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DOI: https://doi.org/10.1023/A:1018922407786