Analytical Methods for Determination of Entacapone in Pharmaceuticals and Urine
Sekar Anubala 1
Ramaiyan Sekar 2  
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Natural Product Chemistry Division, CSIR-Indian Institute of Chemical Technology, Hyderabad-500007, India
Analytical Chemistry Division, CSIR-Indian Institute of Chemical Technology, Hyderabad-500007, India
Organic and Biomolecular Chemistry Division, CSIR-Indian Institute of Chemical Technology, Hyderabad-500007, India
Ramaiyan Sekar   

Analytical Chemistry Division, CSIR-Indian Institute of Chemical Technology, Hyderabad-500007, India
Kommou Nagaiah   

Organic and Biomolecular Chemistry Division, CSIR-Indian Institute of Chemical Technology, Hyderabad-500007, India
Publish date: 2017-10-05
Eurasian J Anal Chem 2015;10(3):150–162
Capillary electrophoresis (CE), high performance thin layer chromatography (HPTLC) and spectrophotometric (SPM) methods were compared for the determination of entacapone in pharmaceutical preparations. And ultrasonication assisted extraction (UAE) coupled with CE determination of cis and trans isomers of entacapone in urine sample was optimized. Resolution of entacapone isomers could not be achieve on RP-HPTLC developed with a native or modified cyclodextrins as a mobile phase additive. Different types aqueous and non-aqueous background electrolytes were tested for the resolution of isomers by CE. Good resolution (Rs ~4.9) was achieved on using a non-aqueous background electrolyte (NBGE). Tailing and concentration dependent migration were observed on silica gel HPTLC plates, due to strong adsorption of entacapone. However, the plate developed with tetrahydrofuran (THF), a good baseline separation was achieved. Good recovery of entacapone was achieved in tablet dosage by using non-aqueous extraction solvent system (NAES). All the methods (SPM, HPTLC and CE) the correlation coefficient (R2) were > 0.9993. SPM method is found be simple, convenient and faster than HPTLC and CE for the determination of entacapone in tablet dosage forms. However, the CE method alone found to be useful for separation and determination of cis and trans isomer in tablets and urine samples and it is simple, fast, cost-effective and efficient.
Männistö PT, Ulmanen I, Lundström K, Taskinen J, Tenhunen J, Tilgmann C, Kaakkola S. (1992) Characteristics of catechol O-methyl-transferase (COMT) and properties of selective COMT inhibitors. Prog. Drug Res. 39: 291.
Doshi AS, Upadhyay KJ, Mehta TN and Nada N (2009) Development and application of a high-performance liquid chromatographic method for the determination of in vitro drug release of levodopa, carbidopa, and entacapone from a tablet formulation. J. AOAC. 92:394.
Issa YM, Hassoun MEM and Zayed AG (2011) Application of high performance liquid chromatographic method for the determination of levodopa, carbidopa, and entacapone in tablet dosage forms.J. Liq. Chromatogr. Relat. Technol. 34: 2433.
Paim C, Goncalves H, Miron D, Sippel J and Steppe M (2007) Stability-Indication LC Determination of Entacapone in Tablets. Chromatographia, 65: 595.
Paim CS, Gonçalves H, Lange A, Miron D and Steppe.M (2008) Validation of UV spectrophotometric method for quantitative determination of entacapone in tablets using experimental design of Plackett-Burman for robustness evaluation and comparison with HPLC. Anal. Lett. 41: 571.
Abasq M.-L, Courtel P and Burgot G (2008) Determination of entacapone by differential pulse polarography in pharmaceutical formulation. Anal. Lett., 41: 56.
Lehtonen P, Laine LM and Wikberg T (1999) Separation of the glucuronides of entacapone and its (Z)-isomer in urine by micellar electrokinetic capillary chromatography.J. Chromatogr. B 721: 127.
Lehtonen P, Lehtinen S, Laine LM and Wikberg T (1999) Micellar electrokinetic capillary chromatography method for direct determination of glucuronides of entacapone and its (Z)-isomer in human urine. J. Chromatogr. A 836: 173.
Karlsson M and Wikberg T (1992) Liquid-chromatographic determination of a new catechol-O-methyltransferase inhibitor, entacapone, and its Z-isomer in human plasma and urine. J. Pharm. Biomed. Anal. 10: 593.
Yadav M, Dixit P, Trivedi V, Gandhi A, Senger A, Guttikar S, Singhal P. and Shrivastav PS (2009) Chromatographic separation of (E)- and (Z)-isomers of entacapone and their simultaneous quantitation in human plasma by LC-ESI-MS/MS. J.Chromatogr. B 877: 533.
Sekar R and Azhaguvel S (2004) Indirect photometric assay determination of gabapentin in bulk drug and capsules by capillary electrophoresis.J. Pharm. Biomed. Anal. 36: 663.
Azhagvuel S and Sekar R (2007) Method development and validation for the simultaneous determination of cetirizine dihydrochloride, paracetamol, and phenylpropanolamine hydrochloride in tablets by capillary zone electrophoresis. J. Pharm. Biomed. Anal. 43: 873.
Sekar R and Azhaguvel S (2008) MEKC determination of antiretroviral reverse transcriptase inhibitors lamivudine, stavudine, and nevirapine in pharmaceutical formulations. Chromatographia 67: 389.
Sekar R and Azhagvuel S (2005) Simultaneous determination of HIV-protease inhibitors lamivudine and zidovudine in pharmaceutical formulations by micellar electrokinetic chromatography. J. Pharm. Biomed. Anal. 39:653.
Hynnila HK, Raanaa K, Taskinen J and Kostiainen R (2000) Direct analysis of nitrocatechol-type glucuronides in urine by capillary electrophoresis–electrospray ionisation mass spectrometry and tandem mass spectrometry. J. Chromatogr., B, 749:253.
Regueiro J, Llompart M, Garcia-Jares C. Garcia-Monteagudo JC and Cela R (2008) Ultrasound-assisted emulsification–microextraction of emergent contaminants and pesticides in environmental waters. J. Chromatogr., A 1190:27-38.
Luque de Castro MD and Priego-Capote F(2007) Ultrasound-assisted preparation of liquid samples. Talanta, 72: 321.
In Analytical Applications of Ultrasound, 1st ed. (2007) Elsevier: Amsterdam, The Netherlands, Vol. 26.
Fontana AR, Patil SH, Banerjee K and Altamirano JC (2010) Ultrasound-Assisted Emulsification Microextraction for Determination of 2,4,6-Trichloroanisole in Wine Samples by Gas Chromatography Tandem Mass Spectrometry. J. Agric. Food Chem. 58:4576.
UGent DL, Goryacheva I, UGent CVP and UGent SDS (2011). Thin-layer chromatography of aflatoxins and zearalenones with beta-cyclodextrins as mobile phase additives. World Mycotoxin J 4: World Mycotoxin J. 113.
Zhang SJ, Zheng XM and Hu WX. Methyl (1H-pyrrol-2-ylcarbonyl­amino)acetate, Acta Crystalographica Section E Structure Reports Online. Oct 1, (2009) 65(Pt) 10:o2351, doi: 10.1107/S1600536809035132).
Feigenbaum A (1986) Hydrogen bonding and retention on silica: A concept illustrated by TLC chromatography of nitrophenols. J.Chem.Education 63: 815.
Anubala S, Sekar R and Nagaiah K (2014) Development and validation of an analytical method for the separation and determination of major bioactive curcuminoids in Curcuma longa rhizomes and herbal products using non-aqueous capillary electrophoresis. Talanta, 123:10-17.
Fillet M, Servais AC and Crommen J (2003) Effects of background electrolyte composition and addition of selectors on separation selectivity in nonaqueous capillary electrophoresis. Electrophoresis 24:1499.
Riekkola ML (2002) Recent advances in nonaqueous capillary electrophoresis, Electrophoresis, 23:3865.