Abstract
Introduction: This study introduces an effective strategy, which combines high performance liquid chromatography coupled with diode array detection (HPLC-DAD) with multivariate calibration methods for the simultaneous determination of paracetamol (PAR), pseudoephedrine HCl (PSE), dextromethorphan HBr (DEX) and doxylamine succinate (DOX) along with sweetener saccharin (SAC) in syrup formulation.
Methods: PLS-2 and PCR calibration algorithms were selected for data processing. Based on the strategy, all target analytes were rapidly quantified within 5.3 min under the simple isocratic elution (water: methanol, 20/80, v/v) without a complete separation. The performances of the proposed methods were confirmed by analyzing a series of synthetic solutions including different concentrations of analytes.
Results: The average recovery values were in the range of 100.33 to 103.70%, and the REP (relative error of prediction) values ranged from 1.96 to 4.36% showed that these methods could provide satisfactory predictions.
Conclusion: Novel HPLC methods coupled with PLS and PCR algorithm enable a simple, fast and low-cost analysis of similar pharmaceutical products for simultaneous determination of the target compounds.
Keywords: Multivariate calibration, HPLC-DAD, multicomponent analysis, saccharin, syrup, paracetamol.
Graphical Abstract
[1]
Conaghan, P.G.; Arden, N.; Avouac, B.; Migliore, A.; Rizzoli, R. Safety of paracetamol in osteoarthritis: What does the literature say? Drugs Aging, 2019, 36(Suppl. 1), 7-14.
[http://dx.doi.org/10.1007/s40266-019-00658-9] [PMID: 31073920]
[http://dx.doi.org/10.1007/s40266-019-00658-9] [PMID: 31073920]
[2]
Laccourreye, O.; Werner, A.; Giroud, J.P.; Couloigner, V.; Bonfils, P.; Bondon-Guitton, E. Benefits, limits and danger of ephedrine and pseudoephedrine as nasal decongestants, Eur; Ann; Otorhinolary, 2015, p. 132.
[3]
Olives, T.D.; Boley, S.P.; LeRoy, J.M.; Stellpflug, S.J. Ten years of robotripping: Evidence of tolerance to dextromethorphan hydrobromide in a long-term user. J. Med. Toxicol., 2019, 15(3), 192-197.
[http://dx.doi.org/10.1007/s13181-019-00706-1] [PMID: 30903576]
[http://dx.doi.org/10.1007/s13181-019-00706-1] [PMID: 30903576]
[4]
Yehia, A.M.; Essam, H.M. Development and validation of a generic high-performance liquid chromatography for the simultaneous separation and determination of six cough ingredients: Robustness study on core-shell particles. J. Sep. Sci., 2016, 39(17), 3357-3367.
[http://dx.doi.org/10.1002/jssc.201600438] [PMID: 27404374]
[http://dx.doi.org/10.1002/jssc.201600438] [PMID: 27404374]
[5]
Čakar, M.; Popovic, G. Determination of saccharin in pharmaceuticals by high performance thin layer chromatography. J. Serb. Chem. Soc., 2006, 71, 669-676.
[http://dx.doi.org/10.2298/JSC0606669C]
[http://dx.doi.org/10.2298/JSC0606669C]
[6]
Katsarov, P.; Gergov, G.; Alin, A.; Pilicheva, B.; Al-Degs, Y.; Simeonov, V.; Kassarova, M. Advanced spectrophotometric chemometric methods for resolving the binary mixture of doxylamine succinate and pyridoxine hydrochloride. Acta Pharm., 2018, 68(1), 61-73.
[http://dx.doi.org/10.2478/acph-2018-0008] [PMID: 29453910]
[http://dx.doi.org/10.2478/acph-2018-0008] [PMID: 29453910]
[7]
Sebaiy, M.M.; El-Adl, S.M.; Mattar, A.A. Different techniques for overlapped UV spectra resolution of some co-administered drugs with paracetamol in their combined pharmaceutical dosage forms. Spectrochim. Acta A Mol. Biomol. Spectrosc., 2020, 224117429
[http://dx.doi.org/10.1016/j.saa.2019.117429] [PMID: 31394394]
[http://dx.doi.org/10.1016/j.saa.2019.117429] [PMID: 31394394]
[8]
Zhang, L.; Hu, Q.; Chen, G.; Fang, Y. Simultaneous determination of the active ingredients in composite pseudoephedrine hydrochloride tablets by capillary electrophoresis. Anal. Chim. Acta, 2000, 424, 257-262.
[http://dx.doi.org/10.1016/S0003-2670(00)01117-X]
[http://dx.doi.org/10.1016/S0003-2670(00)01117-X]
[9]
Cunha, R.R.; Chaves, S.C.; Ribeiro, M.M.; Torres, L.M.; Muñoz, R.A.; Dos Santos, W.T.; Richter, E.M. 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., 2015, 38(10), 1657-1662.
[http://dx.doi.org/10.1002/jssc.201401387] [PMID: 25773878]
[http://dx.doi.org/10.1002/jssc.201401387] [PMID: 25773878]
[10]
Youssef, S.H.; Mohamed, D.; Hegazy, M.A.M.; Badawey, A. Analytical methods for the determination of paracetamol, pseudoephedrine and brompheniramine in Comtrex tablets. BMC Chem, 2019, 13(1), 78.
[http://dx.doi.org/10.1186/s13065-019-0595-6] [PMID: 31384825]
[http://dx.doi.org/10.1186/s13065-019-0595-6] [PMID: 31384825]
[11]
Dong, Y.M.; Li, N.; An, Q.; Lu, N.W. A novel nonionic micellar liquid chromatographic method for simultaneous determination of pseudoephedrine, paracetamol, and chlorpheniramine in cold compound preparations. J. Liq. Chromatogr. Relat. Technol., 2015, 38, 251-258.
[http://dx.doi.org/10.1080/10826076.2014.903850]
[http://dx.doi.org/10.1080/10826076.2014.903850]
[12]
Palabiyik, I.M.; Onur, F. The simultaneous determination of phenylephrine hydrochloride, paracetamol, chlorpheniramine maleate and dextromethorphan hydrobromide in pharmaceutical preparations. Chromatographia, 2007, 66, 93-96.
[http://dx.doi.org/10.1365/s10337-007-0324-5]
[http://dx.doi.org/10.1365/s10337-007-0324-5]
[13]
Dönmez, Ö.A.; Aşçı, B.; Dinç-Zor, Ş.; Çakır, A.A. Simultaneous quantitative analysis of ephedrine HCl, guaifenesin, and some synthetic additives in syrups by RP-HPLC using Box-Behnken design. Lat. Am. J. Pharm., 2018, 37, 85-94.
[14]
Adjekum, A.; Kebede, R. Analysis of dextromethorphan, guaifenesin, benzoate, and saccharin in cough syrup using high- performance liquid chromatography. Concordia College J. Anal. Chem., 2011, 2, 1-5.
[15]
Vistuba, J.P.; Dolzan, M.D.; Vitali, L.; de Oliveira, M.A.; Micke, G.A. Sub-minute method for simultaneous determination of aspartame, cyclamate, acesulfame-K and saccharin in food and pharmaceutical samples by capillary zone electrophoresis. J. Chromatogr. A, 2015, 1396, 148-152.
[http://dx.doi.org/10.1016/j.chroma.2015.03.070] [PMID: 25895731]
[http://dx.doi.org/10.1016/j.chroma.2015.03.070] [PMID: 25895731]
[16]
Dinç-Zor, Ş.; Dönmez, Ö.A.; Aşçı, B.; Pingo, E. Chemometric optimization of an HPLC method for the simultaneous analysis of a multi component drug product by the help of central composite design. Microchem. J., 2020, 104322, 152.
[http://dx.doi.org/10.1016/j.microc.2019.104322]
[http://dx.doi.org/10.1016/j.microc.2019.104322]
[17]
Wang, T.; Wu, H.L.; Xie, L.X.; Liu, Z.; Long, W.J.; Cheng, L.; Ding, Y.J.; Yu, R.Q. Simultaneous and interference-free determination
of eleven non-steroidal anti-inflammatory drugs illegally added
into Chinese patent drugs using chemometrics-assisted HPLCDAD
strategy. Sci. China Chem., 2018, 61, 739-749.
[18]
Bro, R. Review on multiway analysis in chemistry-2000-2005. Crit. Rev. Anal. Chem., 2006, 36, 279-293.
[http://dx.doi.org/10.1080/10408340600969965]
[http://dx.doi.org/10.1080/10408340600969965]
[19]
Mortera, P.; Zuljan, F.A.; Magni, C.; Bortolato, S.A.; Alarcón, S.H. Multivariate analysis of organic acids in fermented food from reversed-phase high-performance liquid chromatography data. Talanta, 2018, 178, 15-23.
[http://dx.doi.org/10.1016/j.talanta.2017.09.005] [PMID: 29136806]
[http://dx.doi.org/10.1016/j.talanta.2017.09.005] [PMID: 29136806]
[20]
Escandar, G.M.; Olivieri, A.C. Multi-way chromatographic calibration-A review. J. Chromatogr. A, 2019, 1587, 2-13.
[http://dx.doi.org/10.1016/j.chroma.2019.01.012] [PMID: 30651205]
[http://dx.doi.org/10.1016/j.chroma.2019.01.012] [PMID: 30651205]
[21]
Olivieri, A.C. Analytical figures of merit: from univariate to multiway calibration. Chem. Rev., 2014, 114(10), 5358-5378.
[http://dx.doi.org/10.1021/cr400455s] [PMID: 24645983]
[http://dx.doi.org/10.1021/cr400455s] [PMID: 24645983]
[22]
Soares, P.K.; Marcheafave, G.G.; de Araújo Gomes, A.; Scarminio, I.S.; Bruns, R.E. Mixture design PARAFAC HPLC-DAD metabolomic fingerprints of fractionated organic and basic extracts from Erythrina speciosa Andrews leaves. Chromatographia, 2018, 81, 1189-1200.
[http://dx.doi.org/10.1007/s10337-018-3554-9]
[http://dx.doi.org/10.1007/s10337-018-3554-9]
[23]
Ghafghazi, S.; Moini Zanjani, T.; Vosough, M.; Sabetkasaei, M. Interference-free determination of carbamazepine in human serum using high performance liquid chromatography: A comprehensive research with three-way calibration methods. Iran. J. Pharm. Res., 2017, 16(1), 120-131.
[PMID: 28496467]
[PMID: 28496467]
[24]
Wu, H.L.; Li, Y.; Yu, R.Q. Recent developments of chemical multiway calibration methodologies with second‐order or higher‐order advantages. J. Chemometr., 2014, 28, 476-489.
[http://dx.doi.org/10.1002/cem.2570]
[http://dx.doi.org/10.1002/cem.2570]
[25]
Zhao, Y.; Yuan, Y.; Chen, J.; Li, M.; Pu, X. Chemometrics-enhanced high performance liquid chromatography strategy for simultaneous determination on seven nitroaromatic compounds in environmental water. Chemom. Intell. Lab. Syst., 2018, 174, 149-155.
[http://dx.doi.org/10.1016/j.chemolab.2017.10.022]
[http://dx.doi.org/10.1016/j.chemolab.2017.10.022]
[26]
Zissis, K.D.; Brereton, R.G.; Dunkerley, S.; Escott, R.E. Two-way, unfolded three-way and three-mode partial least squares calibration of diode array HPLC chromatograms for the quantitation of low-level pharmaceutical impurities. Anal. Chim. Acta, 1999, 384, 71-81.
[http://dx.doi.org/10.1016/S0003-2670(98)00844-7]
[http://dx.doi.org/10.1016/S0003-2670(98)00844-7]
[27]
Dinç, E.; Büker, E. Parallel factor analysis and trilinear partial least squares applied to the UPLC-PDA data array for the quantification of brimonidine tartrate and timolol maleate in an eye drop formulation. J. Liq. Chromatogr. Relat. Technol., 2016, 39, 374-383.
[http://dx.doi.org/10.1080/10826076.2016.1174941]
[http://dx.doi.org/10.1080/10826076.2016.1174941]
[28]
Dönmez, Ö.A.; Dinç-Zor, Ş.; Aşçı, B.; Şen, E. Simultaneous HPLC-DAD determination of pseudoephedrine HCl, sodium benzoate, sunset yellow, and methyl paraben in syrup preparation by use of partial least squares and principal component regression. J. Liq. Chromatogr. Relat. Technol., 2019, 42, 648-653.
[http://dx.doi.org/10.1080/10826076.2019.1647543]
[http://dx.doi.org/10.1080/10826076.2019.1647543]
[29]
Brereton, R.G. Multilevel multifactor designs for multivariate calibration. Analyst (Lond.), 1997, 122, 1521-1529.
[http://dx.doi.org/10.1039/a703654j]
[http://dx.doi.org/10.1039/a703654j]
[30]
Brereton, R.G. Chemometrics: Data Analysis for the Laboratory and Chemical Plant; Wiley: Chichester, 2003.
[http://dx.doi.org/10.1002/0470863242]
[http://dx.doi.org/10.1002/0470863242]
Article Metrics
10
1