STABILITY-INDICATING LIQUID CHROMATOGRAPHY METHOD FOR THE DETERMINATION OF PENTOXYVERINE CITRATE AND ITS DEGRADANT
Keywords:
RP-HPLC, Pentoxyverine citrate, pH-rate profile, Britton-Robinson bufferAbstract
Objectives: The objectives of this research were to develop and validate a HPLC method for determination of Pentoxyverine citrate (PNX) and its degradant (DG).
Methods: Forced degradation studies were performed on bulk sample using alkaline (0.1M sodium hydroxide) and acid (1M hydrochloric acid. The proposed method was based on using a 150 x 4.6 mm (i. d.) (Luna, Phenomenex, Torrance, CA, USA) (5 µm particle size) reversed phase C18 column with mobile phase consisting of a mixture of methanol-10 mM sodium dihydrogen phosphate pH 4 in ratio of (60:40, v/v) and UV detection at 230 nm with flow rate of 1 mL min-1.
Results: The linear calibration range was between 10-40 mg ml-1and 10-40 mg ml-1for PNX and DG respectively. The method was found to be accurate with 100.23% and 100.07% recovery for PNX and DG respectively. The limit of detection (LOD) was found to be 3.79 x10-2μg ml-1 and 4.24 x10-2μg ml-1 for PNX and DG respectively, while the limit of quantification (LOQ) was found to be 12.62 x10-2μg ml-1 and 14.12 x10-2μg ml-1 for PNX and DG respectively. PNX was found to be most stable at a pH of 5.7.
Conclusion: The validation study of the proposed method was successfully carried out and the method was found to be suitable and economic for routine determination of PNX in pharmaceutical syrup, without any interference from the excipients, and in the presence of its acidic and alkaline degradation products.
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References
The British Pharmacopoeia. Her Majesty’s Stationery Office. London; 2010. p. 1638–9.
Sweetman SC. Martindale–The complete drug reference.36thed. London,UK: Vol. 1 The Pharmaceutical Press; 2009. p. 1567–8.
Weclawska K, Regosz A. Colorimetric determination of pentoxyverine citrate in some pharmaceutical preparations. Die Pharmazie 1987;42(7):483–4.
H Hopkala, L Przyborowski, J Flieger. Selective liquid and (vinyl-chloride) pentoxyverine membrane electrodes-their preparation and use for the potentiometric determination of pentoxyverine citrate. Anal Lett 1994;27 (12):2223–38.
Fan Yin. Capacitive sensors using electropolymerized o-phenylenediamine film doped with ion-pair complex as selective elements for the determination of pentoxyverine. Talanta 2004;63(3):641–6.
LI Ping, XU Ying, YANG Sheng-rong. First derivative UV spectrophotometry determination of pentoxyverine citrate sugar-coated tablets. Chin J Pharm Anal 1989;9(2):109.
Wen Xia. Second derivative spectrophotometric determination of pentoxyverine citrate tablets. West Chin J Pharm Sci 2000;15(5):385-6.
Huizhong Zhang, FeiNie, Jiuru Lu. Flow injection chemiluminescence method for the determination of pentoxyverine citrate based on NCS-dichlorofluorescein post-chemiluminescence reaction. Spectro Chim Acta A Mol Biomol Spectrosc 2009;72(4):858–62.
Yingju Liu, Wen Pan, Qian Liu, Shouzhuo Yao. Study on the enhancement of Ru(bpy)3(2+) electrochemiluminescence by nanogold and its application for pentoxyverine detection. Electrophoresis 2005;26(23):4468– 77.
EA Gad-Kariem, MA Abounassif. Determination of pentoxyverine in cough preparations by high performance liquid chromatography. J Liq Chrom Relat Technol 1997;20(18):3049–59.
TIAN Zhao-hong, LIANG Zhu-hong. HPLC determination of pentoxyverine citrate tablets. Northwest Pharm J 2008;23(1):4.
Ke-Hua Yu, Jin-Hua Wen, Fu-Gen Nie, Yu-Qing Xiong. Quantification of pentoxyverine citrate in human plasma by LC-ESI/MS method and its application. Acta Pharm Sin 2009;44(12):1402–5.
Jinhua Wen, Hong Zhang, Chunhua Xia, Xiao Hu, Wenwei Xu, Xiaohua Cheng, et al. A sensitive liquid chromatography-electrospray ionization-mass spectrometry method for the simultaneous determination of pentoxyverine citrate and guaifenesin in human plasma-application to pharmacokinetic and bioequivalence studies. Biomed Chromatogr 2010;24(4):351–7.
Ozlem Aksu Dönmez, Bürge Aşçi, Abdürrezzak Bozdoğan, Sidika Sungur. Simultaneous determination of potassium guaiacolsulfonate, guaifenesin, diphenhydramine HCl and carbetapentane citrate in syrups by using HPLC-DAD coupled with partial least squares multivariate calibration. Talanta 2011;83(5):1601–5.
F Westphal, ThJunge, L Radünz, J Stegk, G Rochholz. Characterization of pentoxyverine metabolites in urine using GC/MS after intoxication with Silomat cough drops. Forensic Sci Int 2012;215(1-3):124-35.
Dina A. Gawad, Tarek S Belal. HPLC-DAD stability indicating determination of pentoxyverine citrate. Application to degradation kinetics and assay of syrup dosage form. Arabian J Chem 2013.
ICH. Stability Testing of New Drug Substances and Products, International Conference on Harmonization, Geneva; 1993.
M Brezina, P Zuman. editors. Polarography in Medicine, Biochemistry and Pharmacy. NewYork: Interscience Publishers; 1958. p. 731.
The European Agency for the Evaluation of Medical Products. ICH Topic Q 2B Note for Guidance on Validation of Analytical Procedures: Methodology CPMP/ICH/281/95, 1996.