Use of Infrared and Ultraviolet Spectroscopy for Galantamine Hydrobromide Assay in Pharmaceuticals and Spiked Human Urine with an Emphasis on Forced Degradation Study

Galantamine hydrobromide (GHB) is an anti-Alzheimer’s drug and a reversible acetylcholinesterase inhibitor. Two simple, sensitive and stability-indicating ultraviolet (UV) spectrophotometric methods were developed and validated for the determination of GHB in pharmaceuticals and a spiked human urine sample. In Method A, the absorbance of the GHB solution in 0.1 M acetic acid (HOAc) was measured at 293 nm. The drug exhibited the same absorbance maximum in 0.1 M hydrochloric acid (HCl), which served as the basis for Method B. Good linearity was ensured over the concentration range of 0.8–80 µg/mL GHB, with correlation coefficients of 0.9807 and 0.9988 for methods A and B, respectively, and the corresponding limits of detection were 0.1477 and 0.3082 µg/mL, while the limits of quantification were 0.4476 and 0.9340 µg/mL, indicating high sensitivity. The Sandell sensitivity values were calculated to be 0.1208 µg/cm² for method A and 0.1175 µg/cm² for method B. Accuracy and precision studies showed low relative error, and %RSD values were below 2%. Robustness was confirmed by deliberate variation of the analytical wavelength by ±2 nm without significant changes in absorbance, while ruggedness studies demonstrated consistent results across different analysts and instruments. Assay of tablet formulations using the standard-addition method yielded the mean percentage recoveries of 98.45 and 100.31% in methods A and B, indicating excellent selectivity. The successful application of the proposed methods to a spiked human urine sample confirmed their biological applicability. Forced degradation studies established the stability-indicating nature of the methods, revealing significant degradation under acidic conditions and good stability under thermal stress, which was further supported by observations in FTIR spectral analysis. The developed methods are rapid, cost-effective and reliable, making them suitable for routine quality control and therapeutic monitoring of GHB.

1. D. D. Tsvetkova, S. A. Ivanova, D. P. Obreshkova, V. B. Petkova, P. Atanasov, P. D. Yordanova-Laleva, A. S. Pashev, World J. Pharm. Pharm. Sci., 9, No. 2, 1–19 (2020).

2. A. V. Patel, V. J. Patel, A. V. Patel, J. B. Dave, C. N. Patel, J. Pharm. Biomed. Sci., 5, No. 4, 314–317 (2013).

3. V. Zarotsky, J. J. Sramek, N. R. Cutler, Am. J. Health Syst. Pharm., 60, No. 5, 446–452 (2003).

4. S. Lilienfeld, CNS Drug Rev., 8, No. 2, 159–176 (2002).

5. C. V. R. Blacker, D. T. Greenwood, K. A. Wesnes, R. Wilson, C. Woodward, I. Howe, T. Ali, JAMA, 292, No. 10, 1195–1204 (2004).

6. United States Pharmacopeia. Galantamine hydrobromide monograph. In: USP 32–NF 27. Rockville (MD): U.S. Pharmacopeial Convention, 2476–2480 (2009).

7. M. J. Culzoni, R. Q. Aucelio, G. M. Escandar, Talanta, 82, No. 2, 325–332 (2010).

8. H. N. Patel, A. V. Patel, V. J. Patel, J. B. Dave, C. N. Patel, J. Chem. Pharm. Res., 2, No. 2, 44–49 (2010).

9. S. Hemambika, K. Raghu Babu, N. Annapurna, Int. J. Res. Chem. Environ., 7, No. 3, 46–53 (2017).

10. N. Taşpınar, İ. Bulduk, Aegean J. Med. Sci., 2, 58–64 (2022).

11. N. Sanli, İ. Bulduk, H. Ozkurt, S. Sanli, S. A. Ozkan, J. Pharm. Biomed. Anal., 134, 174–183 (2017).

12. M. Cuartero, M. S. García, F. García-Cánovas, J. A. Ortuño, Talanta, 110, 8–14 (2013).

13. M. Noetzli, N. Ansermot, M. Dobrinas, C. B. Eap, J. Pharm. Biomed. Anal., 64-65, 16–25 (2012).

14. E. Ozdemir, S. Tatar Ulu, Luminescence, 32, No. 4, 1–5 (2017).

15. M. J. Culzoni, R. Q. Aucelio, G. M. Escandar, Anal. Chim. Acta, 740, 27–35 (2012).

16. J. Maláková, M. Nobilis, Z. Svoboda, M. Lísa, M. Holčapek, J. Kvě tina, J. Klimeš, V. Palička, J. Chromatogr. B, 853, No. 1-2, 265–274 (2007).

17. M. Petrocheilou, V. Samanidou, L. Kovatsi, M. Tsolaki, I. Papadoyannis, J. Appl. Bioanal., 3, No. 4, 59–69 (2017).

18. J. Wang, N. Pavurala, X. Xu, Y. S. R. Krishnaiah, Pfaustino, J. Biomed. Chromatogr., 31, No. 10 (2017).

19. Y. S. Park, S. H. Kim, S. Y. Kim, Y. H. Kim, M. H. Lee, S. C. Yang, L. M. Shaw, J. S. Kang, J. Chromatogr. Sci., 50, No. 9, 803–809 (2012).

20. M. Agami, R. A. Shaalan, S. F. Belal, M. A. A. Ragab, Anal. Bioanal. Chem., 413, 6767–6785 (2021).

21. M. Noetzli, E. Choong, N. Ansermot, C. B. Eap, Ther. Drug. Mon., 33, No. 2, 227–238 (2011).

22. D. Tsvetkova, S. Ivanova, J. Adv. Pharm. Ed. Res., 8, No. 4, 9–14 (2018).

23. D. Tsvetkova, S. Ivanova, J. Adv. Pharm. Ed. Res., 9, No. 1, 1–8 (2019).

24. K. B. Patel, A. V. Patel, V. J. Patel, J. B. Dave, C. N. Patel, J. Chem. Pharm. Res., 2, No. 2, 36–43 (2010).

25. D. L. Pavia, G. M. Lampman, G. S. Kriz, Introduction to Spectroscopy, Philadelphia, WB Saunders (1979).

26. P. Y. Bruice, Organic Chemistry, Upper Saddle River, NJ, Prentice Hall (2004).

27. Y. R. Sharma, Elementary Organic Spectroscopy: Principles and Applications, New Delhi, S. Chand (2015).