DEVELOPMENT AND VALIDATION OF ANALYTICAL METHOD FOR QUANTIFICATION OF ACETIC ACID CONTENT IN AMLODIPINE BESYLATE
Objective: To develop and validate a simple and accurate cost-effective titrimetric method according to International Conference Harmonization (ICH) guidelines for acetic acid content in Amlodipine Besylate.
Methods: The titration based on general acid-base reaction to form water and salt. Sodium hydroxide act as a strong base and titrated against weak acid (acetic acid). Phenolphthalein used as an indicator and colorless to pink is the endpoint. Sodium hydroxide is standardized with primary standard potassium hydrogen phthalate.
Results: The method was linear in the range of 0.75 to 30.25 μg/ml with a correlation coefficient 0.9999. Limit of detection (LOD) and limit of quantitation (LOQ) value were found to be 0.61 and 1.85 μg/ml, respectively. The percentage recovery (98.20–99.97%) and percentage relative standard deviation (%RSD) is less than 2% within the acceptable limit of ICH guidelines. The robustness and ruggedness results were excellent. Method is accurate and precise, no interference from excipients.
Conclusion: A new analytical titrimetric method was developed and validated as per ICH guidelines for the determination of acetic acid content in amlodipine. This proposed method applied for routine analysis of acetic acid content in bulk and pharmaceutical formulations of amlodipine besylate.
2. Tripathi KD. Essentials of medical pharmacology. 5th Edition. Jaypee Brothers Medical Publishers (P) Ltd; 2003. p. 488, 496, 497.
3. Dziezak JD. Acids/natural acids and acidulants. 2nd ed. Encyclopedia of food sciences and nutrition; 2003. p. 12–7.
4. Williams FN, Lee JO. Chemical burns. 5th ed. Total Burn Care; 2018. p. 408–13.
5. Mackison FW, Stricoff RS, Partridge LJJr. NIOSH/OSHA-occupational health guidelines for chemical hazards. Vol. 3. DHHS (NIOSH) Publication No. 81–123 Washington, DC: U. S. Government Printing Office; 1981. p. 2.
6. Bingham E, Cohrssen B, Powell CH. Patty's toxicology. 5th ed. Vol. 1-9. John Wiley and Sons. New York, NY; 2001. p. V5, 703.
7. Hikuma M, Kubo T, Yasuda T. Amperometric determination of acetic acid with immobilized trichosporon brassicae. Anal Chimi Acta 1979;109:33–8.
8. Gibson LT, Cooksey BG, Littlejohn D, Tennent NH. A diffusion tube sampler for the determination of acetic acid and formic acid vapours in museum cabinets. Anal Chim Acta 1997;341:11–9.
9. Shui G, Leong LP. Separation and determination of organic acids and phenolic compounds in fruit juices and drinks by high-performance liquid chromatography. J Chromatogr A 2002; 977:89–96.
10. Sundqvist B, Karlsson O, Westermark U. Determination of formic acid and acetic acid concentrations formed during hydrothermal treatment of birch wood and its relation to colour, strength and hardness. Wood Sci-Tech 2006;40:549.
11. Savary BJ, Nunez A. Gas chromatography-mass spectrometry method for determining the methanol and acetic acid contents of pectin using headspace solid-phase microextraction and stable isotope dilution. J Chromatogr A 2003;1017:151–9.
12. Kumar VA, Aravind G, Srikanth I, Srinivasarao A, Raju CD. Novel analytical method development and validation for the determination of residual solvents in amlodipine besylate by gas chromatography. Der Pharma Chem 2012;4:2228–38.
13. International council for harmonization of technical requirements for pharmaceuticals for human use, Impurities: the guideline for residual solvents, ICH Q3C(R7); 2018.
14. United States Food and Drug Administration. Guidance for industry: Validation of analytical procedures: methodology Q2B; 1996.
15. United States Food and Drug Administration. Guideline for industry: text on validation of analytical procedures: ICH Q2A; 1995.
16. International conference on the harmonization of the technical requirements for registration of pharmaceuticals for human use. Validation of analytical procedures: text and methodology ICH Q2(R1); 1996.
17. Sayeeda S, Balaji N. Simultaneous trace level determination of benzene and 1, 2-dichloroethane by GC-HS/GC-MS in several pharmaceutical drug substances. Int J Appl Pharma 2019:11:82–8.
18. Devesh K. Impact of pharmaceutical industries on the environment, health and safety. J Crit Rev 2015;2:25–30.
19. Pol PA, Mehta PP. Titrimetric analysis of ibuprofen bulk drug sample by using urea as a hydrotropic solubilizing agent. Int J Curr Pharm Res 2015;7:76–7.
20. Tambe VD, Tambe VB, Jadhav RS. Evaluation of leucas aspera whole plant extracts for diuretic and laxative property. Asian J Pharm Clin Res 2016;9:118–21.
21. Sampatti P, Preeti M, Bhagwat C. Quantitative analysis of the salicylic acid bulk sample using hydrotropic solubilizing agents. Asian J Pharm Clin Res 2016;9 Suppl 1:168–9.
22. Jennings PA, Mullen CA, Roy Melinda. Titration and pH measurement. In: Encyclopedia of life sciences (ELS). John Wiley and Sons, Ltd: Chichester; 2010. Doi:10.1002/ 9780470015902.a0002700.pub2.