QUANTITATIVE DETERMINATION OF PLATINUM AND PALLADIUM IN DONEPEZIL HYDROCHLORIDE USING INDUCTIVELY COUPLED PLASMA – OPTICAL EMISSION SPECTROSCOPY
Keywords:
ICP-OES, Platinum, Palladium, Donepezil hydrochlorideAbstract
Objective: To develop a precise, accurate, sensitive and selective analytical method using inductively coupled plasma – optical emission spectroscopy (ICP-OES) for the determination of platinum and palladium in Donepezil hydrochloride raw material, a reversible acetyl cholinesterase inhibitor.
Methods: The method developed and validated uses dry ashing for the extraction of platinum and palladium from Donepezil hydrochloride. Ash thus obtained was leached into an acidic solution followed by analysis of platinum and palladium using ICP-OES at wavelength 306.471 nm and 340.458 nm respectively. The method was studied for the various validation parameters including precision, accuracy, linearity, etc. for both the elements.
Results: The method was found to be linear in the wide working range of 0.2 µg/ml to16 µg/ml with a correlation coefficient of 0.9998 for platinum and 0.1µg/ml to 8µg/ml with a correlation coefficient of 0.9999 for palladium. The recoveries of platinum and palladium from the spiked samples of Donepezil hydrochloride at three different spiking levels were found to be in the range of 86.87 – 98.59% for both platinum and palladium. The limit of detection was found as 0.1 µg/ml and 0.05 µg/ml for platinum and palladium respectively while the limit of quantitation was found to be 0.2 µg/ml and 0.1 µg/ml for platinum and palladium.
Conclusion: The results of the validation studies indicate that the proposed method can be used for the simultaneous determination of platinum and palladium in Donepezil hydrochloride to ensure the quality and purity of Donepezil hydrochloride as a raw material for formulating the pharmaceutical formulations.
Â
Downloads
References
Merck. The Merck index. 13thed. Whitehouse Station NJ, USA: Merck and Co Inc; 2001.
http://drugs.com/monograph/donepezil-hydrochloride.html
Kapasi, Joseph. Process for preparation of Donepezil. European patent application. Patent Number: 1386607Al; 2004.
http://www.ema.europa.eu/docs/en_GB/document_library/Scientific_guideline/2009/09/WC500003587.pdf.
http://www.inchem.org/documents/ehc/ehc/ehc125.htm.
Stellman MS. Encyclopaedia of occupational health and safety, 4thed. Geneva: International Labour Office; 1998.
Yajun W, Xiaozheng L. International symposium on safety science and technology health risk of platinum group elements from automobile catalysts. Procedia Eng 2012;45:1004-9.
Yoe JH, Kirkland JJ. Separation of platinum and palladium and their subsequent colorimetric determination with p-nitrosodimethylaniline. Anal Chem 1954;26(8):1335-9.
Kirkland JJ, Yoe JH. Spectrophotometric study of p-nirosodimethylaniline as sensitive colorimetric reagent for platinum. Anal Chem 1954;26(8):1340-4.
Ryan DE. The detection of palladium, platinum and rhodium with p-nitrosodiphenylamine. Analyst 1951;76:167-71.
Tsunenobu S, Masakazu M. Spectrophotometric determination of palladium with erichrome cyanine R. Bull Inst Chem Res Kyoto Univ 1972;50(6):634-43.
Shrivastava KC. Spectrophotometric determination of palladium with methylthymol blue. J Chin Biochem Soc 1974;21:163-6.
Oscar M, Rains TC. Colorimetric determination of palladium with α-Furildoxime. Anal Chem 1955;27(12):1932-4.
Hiroshi O. Photometric determination of traces of metals.4thed. New York: Vol.1 part 2B Wiley; 1989.
Milner OI, Shipman GF. Colorimetric determination of platinum with stannous chloride. Anal Chem 1955;27(9):1476-8.
Piercy FE, Ryan DE. The colorimetric determination of platinum with 5-(p-dimethylaminobabzalidene)-Rhodanine. Can J Chem 1963;41:667-70.
Dong X, Han Y, Hu Q, Chen J, Yang G. Simultaneous determination of palladium, platinum and rhodium by on-line column enrichment and HPLC with 2, 4-dihydroxybenzylidenethiorhodanine as pre-column derivatization reagent. J Braz Chem Soc 2006;17(1):189-93.
www.chem.agilent.com/Library/usermanuals/Public/1500.pdf
International Conference on Harmonization of Technical requirements for Registration of Pharmaceuticals for human use. Validation of Analytical Procedures: Text and methodology ICH Q2 (R1); 2005.