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Development and Validation of Entacapone in Human Plasma by Liquid Chromatography-Tandem Mass Spectrometry
Corresponding Author(s) : Uttam Prasad Panigrahy
Asian Journal of Chemistry,
Vol. 27 No. 12 (2015): Vol 27 Issue 12
Abstract
A novel liquid chromatography tandem mass spectrometry method is developed for the quantitative determination of entacapone in human plasma in positive ion mode and validated using tolcapone as internal standard according to linearity, selectivity, precision, recovery and various stability studies. Sample preparation was accomplished by liquid-liquid extraction technique. The eluted samples were chromatographed on ACE 3 C18 (150 × 4.6 mm, 5 μ) column (Agilent Technologies) using a mobile phase consisting of HPLC grade acetonitrile:10 mM ammonium phosphate (50:50, v/v) with injection volume of 15 μL and a run time of 3 min. The precursor to product ion transitions m/z 305.10 to 242.10 (entacapone) and m/z 272.20 to 212.10 (tolcapone) were used for quantization. The calibration graph of entacapone was linear with r2 > 0.99 over a concentration range of 60.0 ng/mL to 2200.0 ng/mL. CV % of intra- and inter-day precisions were found satisfactory and well within the limits. The drug was found to be stable for the studied parameters and found to be interference free for matrix effect with appreciable recovery. The novelty of the method makes it highly valuable, rapid, selective and sensitive for quantification of entacapone in human plasma and can be used in therapeutic drug monitoring of this drug.
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- G. Sachs, J.M. Shin and C.W. Howden, Aliment. Pharmacol. Ther., 23(s2), 2 (2006); doi:10.1111/j.1365-2036.2006.02943.x.
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- I. Suslu, S. Altinoz and E. Yildiz, FABAD J. Pharm. Sci., 28, 85 (2003).
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- A. Radi, IL Farmaco, 58, 535 (2003); doi:10.1016/S0014-827X(03)00082-X.
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References
G. Sachs, J.M. Shin and C.W. Howden, Aliment. Pharmacol. Ther., 23(s2), 2 (2006); doi:10.1111/j.1365-2036.2006.02943.x.
R. Huber and M. Hartmann, Int. J. Clin. Pharmacol. Ther., 34, S7 (1996).
X.Q. Li and T.B. Andersson, Drug Metab. Dispos., 32, 821 (2004); doi:10.1124/dmd.32.8.821.
S. Tribedi, M. Ananthapur, J.S. Sabitha, R. Mathappan and V.V. Prasanth, Int. J. Pharm. Chem. Sci., 2, 1454 (2013).
N. Rahman, Z. Bano and S.N.H. Azmi, Anal. Sci., 22, 983 (2006); doi:10.2116/analsci.22.983.
I. Suslu, S. Altinoz and E. Yildiz, FABAD J. Pharm. Sci., 28, 85 (2003).
J. Letica, S. Markovi, J. Zirojevi, K. Nikoli and D. Agbaba, J. AOAC Int., 93, 1121 (2010).
N.V.S. Ramakrishna, K.N. Vishwottam, S. Wishu and M. Koteshwara, J. Chromatogr. B, 822, 326 (2005); doi:10.1016/j.jchromb.2005.06.011.
Z. Xie, X. Chen, F. Jin and D. Zhong, J. Chromatogr. Sci., 43, 271 (2005); doi:10.1093/chromsci/43.5.271.
A. Radi, IL Farmaco, 58, 535 (2003); doi:10.1016/S0014-827X(03)00082-X.
A. Radi, J. Pharm. Biomed. Anal., 33, 687 (2003); doi:10.1016/S0731-7085(03)00356-X.
B.V. Noronha, E.H. Bindewald, M.C. de Oliveira, M.A.P. Papi, M.F. Bergamini and L.H. Marcolino-Jr., Mater. Sci. Eng. C, 43, 517 (2014); doi:10.1016/j.msec.2014.07.060.
Y. Dotsikas, C. Apostolou, S. Soumelas, F. Kolocouri, A. Ziaka, C. Kousoulos and Y.L. Loukas, J. AOAC Int., 93, 1129 (2010).
B.R. Challa, S.H. Boddu, B.Z. Awen, B.R. Chandu, C.K. Bannoth, M. Khagga, K. Kanalae and R.P. Shaik, J. Chromatogr. B, 878, 1499 (2010); doi:10.1016/j.jchromb.2010.03.049.