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Optimization of Kinetic Method for the Estimation of N-Acetyl L-Cysteine and Characterization of its Oxidation and Degradation Product by Mass Spectrometry
Corresponding Author(s) : Masoom Raza Siddiqui
Asian Journal of Chemistry,
Vol. 26 No. 10 (2014): Vol 26 Issue 10
Abstract
A simple kinetic spectrophotometric method has been developed and validated for the quantitative analysis of N-acetyl L-cysteine. The proposed method is based on the oxidation of N-acetyl L-cysteine by potassium permanganate. The mechanism of the reaction was studied and the reaction product was subjected to mass spectrometric analysis for characterization. By the spectral analysis it was concluded that the oxidation of N-acetyl L-cysteine resulted in the formation of a disulfides, sulfinic acid and sulphonic acid. Two methods, initial rate and fixed time were adopted to quantitate the drug. The method was validated as per the ICH guidelines. The calibration graph obtained by the current methods was found to be linear in the range of 3.5-77 μg mL–1. The detection limit of the initial rate and the fixed time methods was calculated to be 8.5 × 10–3 and 0.456, respectively while the quantitation limit came out to be 2.59 × 10–3 and 0.140, respectively for the initial rate and fixed time methods.
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- G.S. Kelly, Altern. Med. Rev., 3, 114 (1998).
- Prkić, J. Giljanović and M. Bralić, Int. J. Electrochem. Sci., 6, 5388 (2011).
- W. Banner Jr., M. Koch, D.M. Capin, S.B. Hopf, S. Chang and T.G. Tong, Toxicol. Appl. Pharmacol., 83, 142 (1986); doi:10.1016/0041-008X(86)90331-5.
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- L. Kukoc-Modun and N. Radić, Anal. Sci., 26, 491 (2010); doi:10.2116/analsci.26.491.
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- M.C.G. Alvarez-Coque, M.J.M. Hernandez, R.M.V. Camanas and C.M. Fernandez, Analyst, 114, 975 (1989); doi:10.1039/an9891400975.
- A. Martinovic and N. Radic, Anal. Lett., 40, 2851 (2007); doi:10.1080/00032710701603884.
- Martinovic and N. Radic, Acta Chim. Slov., 56, 503 (2009).
- M. Kolar and D. Dobcnik, Pharmazie, 58, 25 (2003).
- M. Al-Ghannam, A.M. El-Brashy and B.S. Al-Farhan, IL Farmaco, 57, 625 (2002); doi:10.1016/S0014-827X(02)01223-5.
- W. Wu, G. Goldstein, C. Adams, R.H. Matthews and N. Ercal, Biomed. Chromatogr., 20, 415 (2006); doi:10.1002/bmc.583.
- M.P. Bartolomeo and F. Maisano, J. Biomol. Tech., 17, 131 (2006).
- Z.A. Alothman, M.R. Siddiqui, S.M. Wabaidur, H.A. Al-Lohedan, M.S. Ali and M.Z.A. Rafiquee, Asian J. Chem., 25, 4563 (2013); doi:10.14233/ajchem.2013.14067.
- Z.A. Alothman, M.R. Siddiqui and M.A. Khan, Asian J. Chem., 25, 7229 (2013); doi:10.14233/ajchem.2013.14521.
- P. Sami, N. Mariselvi, K. Venkateshwari, A. Sarathi and K. Rajasekaran, J. Chem. Sci., 122, 335 (2010); doi:10.1007/s12039-010-0038-3.
- J. Ermer, J. Pharm. Biomed. Anal., 24, 755 (2001); doi:10.1016/S0731-7085(00)00530-6.
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- G.D. Christian, Analytical Chemistry, John Wiley & Sons, Inc., Singapore, p. 90 (2004).
- M. Abu Eid, Mikrochim. Acta, 129, 91 (1998); doi:10.1007/BF01246854.
- Canada Health Protection Branch, Drugs Directorate Guidelines, Acceptable Methods, Ministry of National Health and Welfare, Draft (1992).
References
G.S. Kelly, Altern. Med. Rev., 3, 114 (1998).
Prkić, J. Giljanović and M. Bralić, Int. J. Electrochem. Sci., 6, 5388 (2011).
W. Banner Jr., M. Koch, D.M. Capin, S.B. Hopf, S. Chang and T.G. Tong, Toxicol. Appl. Pharmacol., 83, 142 (1986); doi:10.1016/0041-008X(86)90331-5.
H. Ottenwa¨lder and P. Simon, Arch. Toxicol., 60, 401 (1987); doi:10.1007/BF00295763.
L. Kukoc-Modun and N. Radić, Anal. Sci., 26, 491 (2010); doi:10.2116/analsci.26.491.
L. Kukoc-modun, N.Radic, Int. J. Anal. Chem., Article ID 140756 (2011); doi: 10.1155/2011/140756.
M.C.G. Alvarez-Coque, M.J.M. Hernandez, R.M.V. Camanas and C.M. Fernandez, Analyst, 114, 975 (1989); doi:10.1039/an9891400975.
A. Martinovic and N. Radic, Anal. Lett., 40, 2851 (2007); doi:10.1080/00032710701603884.
Martinovic and N. Radic, Acta Chim. Slov., 56, 503 (2009).
M. Kolar and D. Dobcnik, Pharmazie, 58, 25 (2003).
M. Al-Ghannam, A.M. El-Brashy and B.S. Al-Farhan, IL Farmaco, 57, 625 (2002); doi:10.1016/S0014-827X(02)01223-5.
W. Wu, G. Goldstein, C. Adams, R.H. Matthews and N. Ercal, Biomed. Chromatogr., 20, 415 (2006); doi:10.1002/bmc.583.
M.P. Bartolomeo and F. Maisano, J. Biomol. Tech., 17, 131 (2006).
Z.A. Alothman, M.R. Siddiqui, S.M. Wabaidur, H.A. Al-Lohedan, M.S. Ali and M.Z.A. Rafiquee, Asian J. Chem., 25, 4563 (2013); doi:10.14233/ajchem.2013.14067.
Z.A. Alothman, M.R. Siddiqui and M.A. Khan, Asian J. Chem., 25, 7229 (2013); doi:10.14233/ajchem.2013.14521.
P. Sami, N. Mariselvi, K. Venkateshwari, A. Sarathi and K. Rajasekaran, J. Chem. Sci., 122, 335 (2010); doi:10.1007/s12039-010-0038-3.
J. Ermer, J. Pharm. Biomed. Anal., 24, 755 (2001); doi:10.1016/S0731-7085(00)00530-6.
Hartmann, J. Smeyers-Verbeke, W. Penninckx, Y. Vander Heyden, P. Vankeerberghen and D.L. Massart, Anal. Chem., 67, 4491 (1995); doi:10.1021/ac00120a011.
G.D. Christian, Analytical Chemistry, John Wiley & Sons, Inc., Singapore, p. 90 (2004).
M. Abu Eid, Mikrochim. Acta, 129, 91 (1998); doi:10.1007/BF01246854.
Canada Health Protection Branch, Drugs Directorate Guidelines, Acceptable Methods, Ministry of National Health and Welfare, Draft (1992).