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Current Analytical Chemistry

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ISSN (Print): 1573-4110
ISSN (Online): 1875-6727

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Research Article

Multivariate UV-Chemometric and HPLC-QbD Method for Simultaneous Estimation of Vardenafil and Dapoxetine in Active Pharmaceutical Ingredients and its Marketed Formulation

Author(s): Mital N. Patel and Charmy S. Kothari*

Volume 16, Issue 3, 2020

Page: [263 - 276] Pages: 14

DOI: 10.2174/1573411014666180501122512

Price: $65

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Abstract

Background: This manuscript focuses on Novel multivariate UV-chemometric method and HPLC-QbD method for simultaneous determination of Vardenafil (VR) and Dapoxetine (DP) in active pharmaceutical ingredient and their marketed formulation. To the best of our knowledge, there is no literature data on multivariate methods for the same.

Methods: The spectrophotometric data were processed by CLS, PCR, PLS and MLR methods in order to determine the active substances, without prior separation from tablet marketed formulation. Analytical figures of merit, such as sensitivity, selectivity, analytical sensitivity, LOD, and LOQ were determined. In HPLC-QbD, four critical factors were selected after screening and boxbehnken design was applied for optimization. Twenty-five experiments were done, and a quadratic model was used for all response variables. Desirability plot, surface plot, design space, and three-dimensional plots were calculated.

Results: For Chemometrics, wavelength range selected was 202 nm - 326 nm at 2 nm intervals, hence 59 wavelength points were selected in such a way that minimum RMSEC and RMSECV values were obtained at multiple wavelengths. HPLC-QbD optimized conditions were; Phenomenex C8 column (250 × 4.6 mm, 5 µm), acetonitrile: buffer (ammonium acetate buffer at pH 2.7 with acetic acid) (40:60, v/v) as a mobile phase at flow rate of 0.9 mL/min, 239 nm wavelength and 20°C temperature.

Conclusion: The developed methods were validated and successfully applied for simultaneous determination of VR and DP in tablet dosage form. The results obtained by UV-Chemometric methods were statistically compared with an HPLC-QbD method, which concludes both the methods can apply for tablet analysis.

Keywords: Chemometrics, figure of merit, quality by design, response surface design, derringer desirability, design space.

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[1]
Kim, M. J. Clinical Pharmacology and Biopharmaceutics Review ( CS-1 ) 2009, 1-5.
[2]
Angulo, J.; Bischoff, E.; Gabancho, S.; Cuevas, P.; Sáenz de Tejada, I. Vardenafil reverses erectile dysfunction induced by paroxetine in rats. Int. J. Impot. Res., 2003, 15(2), 90-93.
[http://dx.doi.org/10.1038/sj.ijir.3900950] [PMID: 12789386]
[3]
McMahon, C.G. Dapoxetine: a new option in the medical management of premature ejaculation. Ther. Adv. Urol., 2012, 4(5), 233-251.
[http://dx.doi.org/10.1177/1756287212453866] [PMID: 23024705]
[4]
Patel, M.N.; Kothari, C.S. Multivariate Approaches for Simultaneous determination of avanafil and dapoxetine by UV chemometrics and HPLC-QbD in binary mixtures and pharmaceutical product. J. AOAC Int., 2016, 99(3), 649-663.
[http://dx.doi.org/10.5740/jaoacint.15-0259] [PMID: 27075270]
[5]
Paghadar, B.; Antala, H.; Tala, P.; Dhudashia, K.; Patel, N. Q-Absorbance Ratio spectrophotometric method for the simultaneous estimation of vardenafil and Dapoxetine Hydrochloride in Their Combined Dosage Form. Int. J. Res. Pharm. Nano Sci., 2013, 2(1), 124-129.
[6]
Patel, P.D.; Makwana, C.J.; Patel, M.D.; Dey, S.; Upadhyay, U.M. Development and validation of analytical method for simultaneous estimation of vardenafil and Dapoxetine HCl in Bulk and in combined dosage form. Int. J. Pharm. Res. Sch., 2014, 3(2), 17-30.
[7]
Chapla, B.; Amin, G.; Pandya, A.; Kakadiya, J.; Shah, N. Simultaneous estimation and validation of vardenafil and dapoxetine hydrochloride in pharmaceutical formulation by thin layer chromatographic densitometric method. Int. Res. J. Pharm., 2012, 3(5), 480-483.
[8]
Baker, M. M.; Belal, T. S.; Mahrous, M. S.; Ahmed, H. M.; Daabees, H. G. High-Performance Liquid Chromatography with Diode Array Detection Method for the Simultaneous Determination of Seven Selected Phosphodiesterase-5 Inhibitors and Serotonin Reuptake Inhibitors Used as Male Sexual Enhancers J. seperation Sci.,, 2016.
[9]
Kishore, K.K.; Rao, C.K.; Reddy, Y.R.K.; Mukkanti, K. A Validated rapid stability-indicating method for the determination of related substances in solifenacin succinate by Ultra-Fast Liquid Chromatography. Am. J. Anal. Chem., 2012, 3, 59-66.
[http://dx.doi.org/10.4236/ajac.2012.31009]
[10]
Rao, D.V.S.; Surendranath, K.V.; Radhakrishnanand, P.; Suryanarayana, M.V.; Raghuram, P. A stability indicating LC Method for Vardenafil HCl. Chromatographia, 2008, 3(9), 829-835.
[11]
Ku, H-Y.; Shon, J-H.; Liu, K-H.; Shin, J-G.; Bae, S.K. Liquid chromatography/tandem mass spectrometry method for the simultaneous determination of vardenafil and its major metabolite, N-desethylvardenafil, in human plasma: application to a pharmacokinetic study. J. Chromatogr. B Analyt. Technol. Biomed. Life Sci., 2009, 877(1-2), 95-100.
[http://dx.doi.org/10.1016/j.jchromb.2008.11.015] [PMID: 19042162]
[12]
Cheng, C.L.; Kang, G.J.; Chou, C.H. Development and validation of a high-performance liquid chromatographic method using fluorescence detection for the determination of vardenafil in small volumes of rat plasma and bile. J. Chromatogr. A, 2007, 1154(1-2), 222-229.
[http://dx.doi.org/10.1016/j.chroma.2007.03.077] [PMID: 17416379]
[13]
Carlucci, G.; Palumbo, P.; Iuliani, P.; Palumbo, G. Development of a method for the determination of vardenafil in human plasma by high performance liquid chromatography with UV detection. Biomed. Chromatogr., 2009, 23(7), 759-763.
[http://dx.doi.org/10.1002/bmc.1181] [PMID: 19296519]
[14]
Ayoub, B.M. Development and validation of simple spectrophotometric and chemometric methods for simultaneous determination of empagliflozin and metformin: Applied to recently approved pharmaceutical formulation. Spectrochim. Acta A Mol. Biomol. Spectrosc., 2016, 168, 118-122.
[http://dx.doi.org/10.1016/j.saa.2016.06.010] [PMID: 27288963]
[15]
Laursen, K.; Frederiksen, S.S.; Leuenhagen, C.; Bro, R. Chemometric quality control of chromatographic purity. J. Chromatogr. A, 2010, 1217(42), 6503-6510.
[http://dx.doi.org/10.1016/j.chroma.2010.08.040] [PMID: 20846660]
[16]
Cela, R.; Ordoñez, E.Y.; Quintana, J.B.; Rodil, R. Chemometric-assisted method development in reversed-phase liquid chromatography. J. Chromatogr. A, 2013, 1287, 2-22.
[http://dx.doi.org/10.1016/j.chroma.2012.07.081] [PMID: 22901328]
[17]
Glavanović, S.; Glavanović, M.; Tomišić, V. Simultaneous quantitative determination of paracetamol and tramadol in tablet formulation using UV spectrophotometry and chemometric methods. Spectrochim; Acta - Part A Mol. Biomol. Spectrosc, 2015, pp. 1-21.
[18]
Harang, V.; Karlsson, A.; Josefson, M. Liquid chromatography method development and optimization by statistical experimental design and chromatogram simulations. Chromatographia, 2001, 54, 703-709.
[http://dx.doi.org/10.1007/BF02492487]
[19]
De Beer, J.O.; Vandenbroucke, C.V.; Massart, D.L.; De Spiegeleer, B.M. Half-fraction and full factorial designs versus central composite design for retention modelling in reversed-phase ion-pair liquid chromatography. J. Pharm. Biomed. Anal., 1996, 14(5), 525-541.
[http://dx.doi.org/10.1016/0731-7085(95)01655-4] [PMID: 8738182]
[20]
Xiong, Y.; Xiao, K.P.; Rustum, A.M. Development and validation of a stability-indicating RP-HPLC method to separate low levels of dexamethasone and other related compounds from betamethasone. J. Pharm. Biomed. Anal., 2009, 49(3), 646-654.
[http://dx.doi.org/10.1016/j.jpba.2008.12.023] [PMID: 19171447]
[21]
Srinubabu, G.; Jaganbabu, K.; Sudharani, B.; Venugopal, K.; Girizasankar, G.; Rao, J.V.L.N.S. Development and validation of a LC method for the determination of pramipexole using an experimental design. Chromatographia, 2006, 64(1-2), 95-100.
[http://dx.doi.org/10.1365/s10337-006-0829-3]
[22]
Garg, L. kumar; Reddy, V. S. Quality by design : Design of experiments approach prior to the Validation of a Stability-Indicating HPLC method for montelukast. Chromatographia, 2013, 2509-2504.
[23]
Garg, L.K.; Sait, S.S.; Krishnamurthy, T.; Kumar, C.H.R.P. Quality by Design (QbD): A practical experimental design approach by blocking and varying certain factors of a Stability-Indicating HPLC method for simultaneous determination of omeprazole and Ketoprofen. J. Liq. Chromatogr. Relat. Technol., 2015, 38(6), 677-686.
[http://dx.doi.org/10.1080/10826076.2014.951766]
[24]
Patel, M.N.; Kothari, C.S. Review on implementation of multivariate approach for forced degradation study and impurity profiling with regulatory considerations. Chromatographia, 2017.
[25]
Hadad, G.M.; El-Gindy, A.; Mahmoud, W.M.M. HPLC and chemometrics-assisted UV-spectroscopy methods for the simultaneous determination of ambroxol and doxycycline in capsule. Spectrochim. Acta A Mol. Biomol. Spectrosc., 2008, 70(3), 655-663.
[http://dx.doi.org/10.1016/j.saa.2007.08.016] [PMID: 17931962]
[26]
Olivieri, A.C.; Faber, N.K.M.; Ferre, J.; Boque, R.; Kalivas, J.H.; Mark, H. Uncertainty Estimation and Figures of Merit for Multivariate Calibration. Pure Appl. Chem., 2006, 78(3), 633-661.
[http://dx.doi.org/10.1351/pac200678030633]
[27]
Sankar, A.S.; Vetrichelvan, T.; Venkappaya, D. Simultaneous estimation of ramipril, acetylsalicylic acid and atorvastatin calcium by chemometrics assisted UV-spectrophotometric method in capsules. Acta Pharm., 2011, 61(3), 283-296.
[http://dx.doi.org/10.2478/v10007-011-0027-1] [PMID: 21945907]
[28]
Patil, A.S.; Pethe, A.M. Quality by Design (QbD) : A New Concept for Development of Quality Pharmaceuticals. Int. J. Pharm. Qual. Assur., 2013, 4(2), 13-19.
[29]
Monks, K.; Molnár, I.; Rieger, H.J.; Bogáti, B.; Szabó, E. Quality by Design: Multidimensional exploration of the design space in high performance liquid chromatography method development for better robustness before validation. J. Chromatogr. A, 2012, 1232, 218-230.
[http://dx.doi.org/10.1016/j.chroma.2011.12.041] [PMID: 22226460]
[30]
Harmonised, I.C.H.; Guideline, T. ICH Harmonised Tripartite Guideline Validation of Analytical Procedures. Text and Methodology, 2014, Q2(R1), 1-13.

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