RAPID ANALYSIS OF CAFFEINE AND PARACETAMOL USING MICRO-LIQUID CHROMATOGRAPHY WITH MIXED MODE MONOLITHIC COLUMN

Authors

  • Kesara Ar-sanork School of Chemistry, Institute of Science, Suranaree University of Technology, 111 University Avenue, Muang District, Nakhon Ratchasima 30000, Thailand.
  • Lalida Wongbuth School of Chemistry, Institute of Science, Suranaree University of Technology, 111 University Avenue, Muang District, Nakhon Ratchasima 30000, Thailand.
  • Chanpen Karuwan Graphene and Printed Electronics for Dual-Use Applications Research Division (GPERD), National Science and Technology Development Agency (NSTDA), Pathum Thani 12120, Thailand.
  • Nakin Surapanich Department of Chemistry, Faculty of Science and Technology, Rajanagarindra Rajabhat University, 22 Maruphong Road, Na Mueang, Muang, Chachoengsao, 24000, Thailand.
  • Prapin Wilairat National Doping Control Centre, Mahidol University, Rama VI Rd, Bangkok 10400, Thailand.
  • Patcharin Chaisuwan School of Chemistry, Institute of Science, Suranaree University of Technology, 111 University Avenue, Muang District, Nakhon Ratchasima 30000, Thailand.

Keywords:

Caffeine, paracetamol, monolithic column, micro-liquid chromatography, triethylamine additive

Abstract

This work developed a simple and rapid micro-liquid chromatographic method using a synthesized monolithic capillary column for analysis of caffeine and paracetamol in pharmaceutical drugs. The monolithic column was synthesized from methacrylic acid and ethylene dimethacrylate monomers. Due to the anionic and hydrophobic properties of the polymeric stationary phase, complete separation of the two compounds was achieved by addition of triethylamine into the acetonitrile-aqueous buffer (pH 10.0) mobile phase using a micro-liquid chromatograph with uv-visible detector. Under the optimal condition, the two compounds were separated in less than 3 min. Good linearity in the concentration range of 1-50 mg/L (r2>0.997) with detection limits of 0.05 mg/L for paracetamol and 0.30 mg/L for caffeine were obtained. The method was successfully applied to the determination of caffeine and paracetamol in drug samples with percent recoveries of 102 and 99, respectively.

References

Acheampong, A., Gyasi, W.O., Darko, G., Apau, J., and Addai Arhin, S. (2016). Validated RP HPLC method for simultaneous determination and quantification of chlorpheniramine maleate, paracetamol and caffeine in tablet formulation. Springer Plus., 5:1-8.

Alves, J.C.L., and Poppi, R.J. (2009). Simultaneous determination of acetylsalicylic acid, paracetamol and caffeine using solid-phase molecular fluorescence and parallel factor analysis. Anal. Chim. Acta., 642:212-216.

Ashour, A., Hegazy, M.A., Abdel-Kawy, M., and ElZeiny, M.B. (2012). Simultaneous spectrophotometric determination of overlapping spectra of paracetamol and caffeine in laboratory prepared mixtures and pharmaceutical preparations using continuous wavelet and derivative transform. J. Saudi Chem. Soc., 19:186-192.

Chaloemsuwiwattanakan, T., Sangcakul, A., Kitiyakara, C., Nacapricha, D., Wilairat, P., and Chaisuwan, P. (2016). Simple and fast analysis of iohexol in human serums using micro-hydrophilic interaction liquid chromatography with monolithic column. J. Sep. Sci., 39:3521-3527.

Chaves, S.C., Aguiar, P.N.C., Torres, L.M.F.C., Gil, E.S., Luz, R.C.S., Damos, F.S., Munoz, R.A.A., Richter, E.M., and Dos Santos, W.T.P. (2015). Simultaneous determination of caffeine, ibuprofen, and paracetamol by flow-injection analysis with multiple-pulse amperometric detection on boron-doped diamond electrode. Electroanalysis., 27:2,785-2,791.

Cunha, R.R., Chaves, S.C., Ribeiro, M.M.A.C., Torres, L.M.F.C., Muñoz, R.A.A., Santos, W.T.P.D., and Richter, E.M. (2015). Simultaneous determination of caffeine, paracetamol, and ibuprofen in pharmaceutical formulations by high-performance liquid chromatography with UV detection and by capillary electrophoresis with conductivity detection. J. Sep. Sci., 38:1,657-1,662.

Diener, H.C., Peil, H., and Aicher, B. (2011). The efficacy and tolerability of a fixed combination of acetylsalicylic acid, paracetamol, and caffeine in patients with severe headache: A post-hoc subgroup analysis from a multicentre, randomized, double-blind, single-dose, placebo controlled parallel group study. Cephalalgia., 31:1,466-1,476.

Dinc, E., Kokdol, G., and Onur, F. (2001). Derivative ratio spectra–zero crossing spectrophotometry and LC method applied to the quantitative determination of paracetamol, propyphenazone and caffeine in ternary mixtures. J. Pharm. Biomed. Anal., 26:769-778.

Gong, L. (2015). Comparing ion-pairing reagents and counter anions for ion-pair reversed-phase liquid chromatography/electrospray ionization mass spectrometry analysis of synthetic oligonucleotides. Rapid Commun. Mass Spectrom., 29:2,402-2,410.

Kartal, M. (2001). LC method for the analysis of paracetamol, caffeine and codeine phosphate in pharmaceutical preparations. J. Pharm. Biomed. Anal., 26:857-864.

Khoshayand, R.M., Abdollahi, H., Shariatpanahi, M., Saadatfard, A., and Mohammadi, M. (2008). Simultaneous spectrophotometric determination of paracetamol, ibuprofen and caffeine in pharmaceuticals by chemometric methods. Spectrochim. Acta, Part A., 70:491-499.

Koblova, P., Sklenarova, H., Brabcova, I., and Solich, P. (2012). Development and validation of a rapid HPLC method for the determination of ascorbic acid, phenylephrine, paracetamol and caffeine using a monolithic column. Anal. Methods., 4:1588-1591.

Kullilow, A.U., and Verushkin, A.G. (2008). Simultaneous determination of paracetamol, caffeine, guaifenesin and preservatives in syrups by micellar LC. Chromatographia., 67:347-355.

Machado Alencar, L., Backes dos Santos, R., de Jesus Guedes, T., Torres Pio dos Santos, W., Batista Gomes de Souza, J., Souza Ferreira, V., and Amorim Bezerra da Silva, R. (2017). Fast and selective simultaneous determination of acetaminophen, aspirin and caffeine in pharmaceutical products by batch injection analysis with multiple pulse amperometric detection. Electroanalysis., 29:296-303.

Mahadevan, S.B.K., McKiernan, P.J, Davies, P., and Kelly, D.A. (2006). Paracetamol induced hepatotoxicity. Arch. Dis. Child., 91:598–603.

Minh, T.T., Phong, N.H., Van Duc, H., and Khieu, D.Q. (2017). Microwave synthesis and voltammetric simultaneous determination of paracetamol and caffeine using an MOF-199-based electrode. J. Mater. Sci., 53:2,453-2,471.

Pakravan, N., Bateman, D.N., and Goddard, J. (2007). Effect of acute paracetamol overdose on changes in serum and urine electrolytes. Br. J. Clin. Pharmacol., 64:824-832.

Pfaunmille, E.L., Paulemond, M. L., Dupper, C.M., and Hage, D.S. (2013). Affinity monolith chromatography: a review of principles and recent analytical applications. Anal. Bioanal. Chem., 405:2,133-2,145.

Pistos, C., and Stewart, J.T. (2004). Assay for the simultaneous determination of acetaminophen–caffeine–butalbital in human serum using a monolithic column. J. Pharm. Biomed. Anal., 36:737-741.

Prasad, C., and Ragan, A. (1994). Use of triethylamine as an ion-pairing reagent. J. Liq. Chromatogr., 17:2,383-2,394.

Samanidou, V.F., and Karageorgou, E.G. (2011). An overview of the use of monoliths in sample preparation and analysis of milk. J. Sep. Sci., 34:2,013-2,025.

Silva, W.P., Silva, L.A.J., Franca, C.H., Sousa, R.M.F., Monoz, R.A.A., and Richter, E.M. (2017). Square-wave voltammetric determination of propyphenazone, paracetamol, and caffeine: comparative study between batch injection analysis and conventional electrochemical systems. Electroanalysis., 29:1,860-1,866.

Straube, A., Aicher, B., Fiebich, B.L., and Haag G. (2011). Combined analgesics in (headache) pain therapy: shotgun approach or precise multi-target therapeutics?. BMC Neurol., 11:1-15.

Svec, F., and Huber, G.C. (2006). Monolithic materials: promises, challenges, achievements. Anal. Chem., 78:2,101- 2,107.

Tefera, M., Geto, A., Tessema, M., and Admassie, S. (2016). Simultaneous determination of caffeine and paracetamol by square wave voltammetry at poly (4-amino-3-hydroxynaphthalene sulfonic acid)-modified glassy carbon electrode. Food Chem., 210:156-162.

Topkafa, M., Ayyildiz, H.F., Memon, F.N., and Kara, H. (2016). New potential humic acid stationary phase toward drug components: Development of a chemometric-assisted RP-HPLC method for the determination of paracetamol and caffeine in tablet formulations. J. Sep. Sci., 39:2,451-2,458.

Wang, A., Sun, J., Feng, H., Gao, S., and He, Z. (2007). Simultaneous determination of paracetamol and caffeine in human plasma by LC–ESI–MS. Chromatographia., 67:281-285.

Zhu, T., and Row, K.H. (2012). Monolithic materials and their applications in HPLC for purification and analysis of bioactive compounds from natural plants: a review. Instrum. Sci. Technol., 40:78-89.

Downloads

Published

2026-08-28

How to Cite

Ar-sanork, K., Wongbuth, L., Karuwan, C., Surapanich, N., Wilairat, P., & Chaisuwan, P. (2026). RAPID ANALYSIS OF CAFFEINE AND PARACETAMOL USING MICRO-LIQUID CHROMATOGRAPHY WITH MIXED MODE MONOLITHIC COLUMN. Suranaree Journal of Science and Technology, 28(2), 030041(1–6). retrieved from https://ph04.tci-thaijo.org/index.php/SUJST/article/view/14903

Issue

Section

Research Article