• MALAK Y. AL BATHISH Department of Pharmaceutical Technology, Faculty of Pharmacy, Beirut Arab University, Beirut, Lebanon
  • AZZA A. GAZY Department of Pharmaceutical Technology, Faculty of Pharmacy, Beirut Arab University, Beirut, Lebanon
  • MARWA K. EL JAMAL Department of Pharmaceutical Technology, Faculty of Pharmacy, Beirut Arab University, Beirut, Lebanon



Methimazole, Spectrophotometric methods, Potassium permanganate, Cerium (IV) nitrate, Methyl orange


Objective: To develop and validate new, selective spectrophotometric colorimetric analytical methods for the quantification of methimazole in its pure form and in its pharmaceutical preparations.

Methods: Method A is based on the oxidation of methimazole with potassium permanganate in alkaline medium, the manganate ion produced was measured at λmax= 610 nm. Method B is a kinetic determination of methimazole using fixed-time method based on the oxidation of methimazole using known excess of cerium (IV) nitrate in acidic medium and assessing the unreacted Ce (IV) by adding a fixed amount of methyl orange and measuring the absorbance of the resultant solution at λmax=507 nm which is equivalent to the unreacted methyl orange. The reaction conditions and analytical parameters are investigated and optimized. Method validation was carried out according to ICH guidelines in terms of linearity, LOD, LOQ, precision, and accuracy.

Results: Beer’s law is obeyed in the range of 1.50–15.00 μg/ml for method A and 0.25–3.00 μg/ml for method B. The developed methods were subjected to the detailed validation procedure. The proposed spectrophotometric methods were applied for the determination of the methimazole in its pure form and in its pharmaceutical formulation. The percentage recoveries were found to be 100.82 % and 99.85 % in the pharmaceutical formulation for the two proposed methods, respectively.

Conclusion: Both developed spectrophotometric methods, considered as green analytical chemistry, were found to be novel, highly selective and can be applied for the quality control of methimazole in its pure form and in its pharmaceutical formulation based on the simplicity, applicability of the parameters, accessibility of the reagents employed and reasonably low time of analysis.


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USP US. Pharmacopoeia-National Formulary [USP 38 NF 33]. Rockville, Md United States Pharmacopeial Conv; 2015.

Garcia MS, Albero MI, Sanchez Pedreno C, Tobal L. Kinetic determination of carbimazole, methimazole and propylthiouracil in pharmaceuticals, animal feed and animal livers. Analyst 1995;120:129–33.

Sanchez Pedreño C, Albero MI, Garcia MS, Rodenas V. Flow-injection spectrophotometric determination of carbimazole and methimazole. Anal Chim Acta 1995;308:457–61.

Dong C, Zhang Y, Guo L, Li Q. Spectrophotometric determination of methimazole in pharmaceutical, serum and urine samples by reaction with potassium ferricyanide-Fe(III). J Anal Chem 2010;65:707–12.

Tu CQ, Wen XR. Indirect determination of methimazole in a pharmaceutical sample by discoloration spectrophotometry using Fe (III)-tiron system. Adv Mater Res 2013;781–784:115–9.

Rahmani A. Sensitive photometric method for the assay of methimazole in pure and pharmaceutical formulations; 2015. p. 64–7.

Chipiso K, Simoyi RH. Kinetics and mechanism of oxidation of methimazole by chlorite in slightly acidic media. J Phys Chem A 2016;120:3767–79.

El-Bardicy MG, El-Saharty YS, Tawakkol MS. Determination of carbimazole and methimazole by first and third derivative spectrophotometry. Spectrosc Lett 1991;24:1079–95.

Min H, Zeng Ping C, Yao C, Cai Xia S, Ru-Qin Y. Quantification of methimazole in plasma and tablet samples by surface-enhanced raman spectroscopy in combination with the multiplicative effects model. Chinese J Anal Chem 2015;43:759–64.

Saleh TA, Al-Shalalfeh MM, Al-Saadi AA. Graphene dendrimer-stabilized silver nanoparticles for the detection of methimazole using surface-enhanced raman scattering with the computational assignment. Sci Rep 2016;6:32185.

Liu X, Yuan H, Pang D, Cai R. Resonance light scattering spectroscopy study of interaction between gold colloid and thiamazole and its analytical application. Spectrochim Acta Part A Mol Biomol Spectrosc 2004;60:385–9.

Economou A, Tzanavaras PD, Notou M, Themelis DG. Determination of methimazole and carbimazole by flow-injection with chemiluminescence detection based on the inhibition of the Cu(II)-catalysed luminol–hydrogen peroxide reaction. Anal Chim Acta 2004;505:129–33.

Sheng Z, Han H, Yang G. A novel method for sensing of methimazole using gold nanoparticle-catalyzed chemiluminescent reaction. Luminescence 2011;26:196–201.

Kong D, Li Q, Jiang J, Xinyu Z, Xuechou Z, Chi Y, et al. Flow injection analysis of thiamazole based on strong Ru(bpy) 3 2+co‐reactant electrochemiluminescence. Luminescence 2015; 30:12–7.

Dong F, Hu K, Han H, Liang J. A novel method for methimazole determination using CdSe quantum dots as fluorescence probes. Microchim Acta 2009;165:195–201.

Farzampour L, Amjadi M. Sensitive turn-on fluorescence assay of methimazole based on the fluorescence resonance energy transfer between acridine orange and silver nanoparticles. J Lumin 2014;155:226–30.

Sun J, Zheng C, Xiao X, Niu L, You T, Wang E. Electrochemical detection of methimazole by capillary electrophoresis at a carbon fiber microdisk electrode. Electroanalysis 2005;17:1675–80.

Wang JP, Tang WW, Fang GZ, Pan MF, Wang S. Development of a biomimetic enzyme-linked immunosorbent assay method for the determination of methimazole in urine sample. J Chinese Chem Soc 2011;58:463–9.

Pan M, Fang G, Lu Y, Kong L, Yang Y, Wang S. Molecularly imprinted biomimetic QCM sensor involving a poly(amidoamine) dendrimer as a functional monomer for the highly selective and sensitive determination of methimazole. Sensors Actuators B Chem 2015;207:588–95.

Aletrari M, Kanari P, Partassides D, Loizou E. Study of the British pharmacopeia method on methimazole (thiamazole) content in carbimazole tablets. J Pharm Biomed Anal 1998;16:785–92.

Hollosi L, Kettrup A, Schramm KW. MMSPE-RP-HPLC method for the simultaneous determination of methimazole and selected metabolites in fish homogenates. J Pharm Biomed Anal 2004;36:921–4.

Kusmierek K, Bald E. Determination of methimazole in urine by liquid chromatography. Talanta 2007;71:2121–5.

Zakrzewski R. Determination of methimazole in pharmaceutical preparations using an HPLC method coupled with an iodine-azide post-column reaction. J Liq Chromatogr Relat Technol 2008;32:383–98.

Zakrzewski R. Determination of methimazole in urine with the iodine-azide detection system following its separation by reversed-phase high-performance liquid chromatography. J Chromatogr B 2008;869:67–74.

Pan M, Wang J, Fang G, Tang W, Wang S. Synthesis and characterization of a molecularly imprinted polymer and its application as SPE enrichment sorbent for determination of trace methimazole in pig samples using HPLC-UV. J Chromatogr B 2010;878:1531–6.

Xi X, Ming L, Liu J. Electrochemical determination of thiamazole at a multi-wall carbon nanotube modified glassy carbon electrode. J Appl Electrochem 2010;40:1449–54.

Yazhen W. Electrochemical determination of methimazole based on the acetylene black/chitosan film electrode and its application to rat serum samples. Bioelectrochemistry 2011;81:86–90.

Kutluay A, Aslanoglu M. Multi-walled carbon nanotubes/electro-copolymerized cobalt nanoparticles-poly(pivalic acid) composite film coated glassy carbon electrode for the determination of methimazole. Sensors Actuators B Chem 2012;171–172:1216–21.

Jalali F, Miri L, Roushani M. Electrocatalytic determination of anti-hyperthyroid drug, methimazole, using a modified carbon-paste electrode. African J Pharm Pharmacol 2013;7:269–74.

Fouladgar M, Mohammadzadeh S. Determination of methimazole on a multiwall carbon nanotube titanium dioxide nanoparticle paste electrode. Anal Lett 2014;47:763–77.

Norouzi P, Gupta VK, Larijani B, Ganjali MR, Faridbod F. A new methimazole sensor based on a nanocomposite of CdS NPs–RGO/IL–carbon paste electrode using differential FFT continuous linear sweep voltammetry. Talanta 2014;127:94–9.

Dorraji PS, Jalali F. Sensitive amperometric determination of methimazole based on the electrocatalytic effect of rutin/multi-walled carbon nanotube film. Bioelectrochemistry 2015;101:66–74.

Si W, Han Z, Lei W, Wu Q, Zhang Y, Xia M, et al. Fast electrochemical determination of imidacloprid at an activated glassy carbon electrode. J Electrochem Soc 2014;161:B9–13.

Rahman N, Anwar N, Kashif M, Hoda MN, Rahman H. Determination of labetalol hydrochloride by kinetic spectrophotometry using potassium permanganate as oxidant. J Mex Chem Soc 2011;55:105–12.

Wahed MGA, Sheikh R El, Gouda AA, Taleb SA. Kinetic spectrophotometric determination of some fluoroquinolone antibiotics in bulk and pharmaceutical preparations. Bull Chem Soc Ethiop 2013;27:329–46.

Reddy KD, Sayanna K, Venkateshwarlu G. Kinetic spectrophotometric determination of drugs based on oxidation by alkaline KMno4. J Appl Chem 2014;6:8–14.

Darwish IA, Khedr AS, Askal HF, Mohamed RM. Application of inorganic oxidants to the spectrophotometric determination of ribavirin in bulk and capsules. J AOAC Int 2006;89:341–51.

Krebs A, Starczewska B, Puzanowska Tarasiewicz H, Sledz J. Spectrophotometric determination of olanzapine by its oxidation with N-bromosuccinimide and cerium (IV) sulfate. Anal Sci 2006;22:829–33.

Abdellatef HE, El-Henawee MM, El-Sayed HM, Ayad MM. Spectrophotometric and spectrofluorimetric methods for the analysis of acyclovir and acebutolol hydrochloride. Spectrochim Acta Part A Mol Biomol Spectrosc 2006;65:997–9.

David IG, David V, Ciucu AA, Ciobanu A. Indirect spectrophotometric determination of neomycin based on the reaction with cerium (IV) sulfate. Department Phys Chem 2010;19:61–8.

ICH. Validation of analytical procedures: text and methodology Q2(R1). International Conference on Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human Use; 2005.

John Rose. Advanced Physicochemical Experiments. Pitman Publishing; 1964.



How to Cite

AL BATHISH, M. Y., A. A. GAZY, and M. K. EL JAMAL. “NOVEL SELECTIVE SPECTROPHOTOMETRIC METHODS FOR THE DETERMINATION OF METHIMAZOLE IN PURE FORM AND IN PHARMACEUTICAL FORMULATION”. International Journal of Pharmacy and Pharmaceutical Sciences, vol. 12, no. 2, Feb. 2020, pp. 62-69, doi:10.22159/ijpps.2020v12i2.35715.



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