Quantitative Spectrophotometric Analysis of Metoclopramide Hydrochloride in Pharmaceutical Tablets via Bromination Reaction
DOI:
https://doi.org/10.67151/rujbas.v1i1.29Keywords:
Metoclopramide hydrochloride, bromate-bromide mixture, methylene blue, spectrophotometry, pharmaceutical tabletsAbstract
This study aimed to suggest and validate a simple and sensitive visible spectrophotometric method for the quantification of metoclopramide hydrochloride (MCPH) in its pure form and pharmaceutical tablets. The method uses bromine generated in situ by the action of an acid on a mixture of bromate and bromide, which acts as an environmentally friendly brominating agent for the bromination of MCPH. It enables a cost-effective analysis while eliminating the handling of hazardous liquid bromine. The method is based on adding a carefully measured excess of bromate-bromide reagent to MCPH solution in an acidic medium. Upon completion of the reaction, the residual bromine is quantified by reacting it with a fixed amount of methylene blue dye, followed by measuring the absorbance at 665 nm. Under optimal conditions, MCPH can be quantified over a concentration range of 1.25–25.0 µg/mL, with a molar absorptivity of 1.032×10⁴ L/mol.cm and a Sandell's sensitivity of 0.0326 µg/cm². Experimental t- and F-values were calculated and compared with critical tabulated values using Student t-test and F-ratio at a 95% confidence level, confirming no significant difference between the official and suggested methods in terms of accuracy and precision. The suggested method was successfully applied for the analysis of MCPH in raw material and tablets, and its reliability was confirmed using a standard addition method.
References
[1] Shakeel F, Shazly GA, Haq N. Solubility of metoclopramide hydrochloride in six green solvents at (298.15 to 338.15) K. Journal of Chemical and Engineering Data. 2014;59(5):1700-3. https://doi.org/10.1021/je500154k DOI: https://doi.org/10.1021/je500154k
[2] Aronson JK. Meyler's side effects of drugs: the international encyclopedia of adverse drug reactions and interactions. 16th ed. Amsterdam: Elsevier Science; 2016.
[3] Demir I, Bulduk I, Darwısh IA, Enginar H. A green approach for metoclopramide quantification in pharmaceutical products: new HPLC and spectrophotometric methods. Scientific Reports. 2024;14:8765. https://doi.org/10.1038/s41598-024-59149-6 DOI: https://doi.org/10.1038/s41598-024-59149-6
[4] Al-Sabha TN, Al-Hamody IA. Spectrophotometric determination of metoclopramide hydrochloride in bulk and in pharmaceutical preparations. Iraqi National Journal of Chemistry. 2006;6(24):561-70.
[5] Wamorkar V, Manjunath SY, Varma MM. Development and validation of UV spectroscopic method for determination of metoclopramide hydrochloride in bulk and tablet formulation. International Journal of Pharmacy and Pharmaceutical Sciences. 2011;3(3):171-4.
[6] Thangamani A, Smith AA, Vedhapriya B. Development of analytical method for metoclopramide using UV-spectrophotometry. International Journal of Pharmaceutical, Chemical and Biological Sciences. 2014;4(3):551-5.
[7] Basheer MY, Kashif AA, Aljaily A, Ibrahim MM, Osman HM. Development and validation of UV-spectroscopic method for assay of metoclopramide hydrochloride in bulk and injectable dosage form. American Journal of Research Communication. 2017;5(3):22-33.
[8] Ahmed NR, Essa MJ, Hamdoon AK. Ultraviolet assay of metoclopramide HCl in pharmaceutical formulations application to content uniformity testing. European Journal of Biomedical and Pharmaceutical Sciences. 2020;7(1):191-95.
[9] Othman NS, Mahmood HS, Khaleel NA. Spectrophotometric and high performance liquid chromatographic methods for determination of metoclopramide in pharmaceutical preparations. Rafidain Journal of Science. 2011;22(3):39-56. DOI: https://doi.org/10.33899/rjs.2011.6510
[10] Khaleel AI, Amine ST, Salih SH. Comparative study for determination of metoclopramide hydrochloride drug by selective electrodes and spectrophotometric methods. Tikrit Journal of Pure Science. 2013;18(1):149-61.
[11] Blazheyevskiy M, Alfred-Ugbenbo D, Mozgova OO, Moroz VP. Determination of metoclopramide hydrochloride in pharmaceutical formulations using N-oxidation caroate. Turkish Journal of Pharmaceutical Sciences. 2022;19(5):589-94. https://doi.org/10.4274/tjps.galenos.2021.33733 DOI: https://doi.org/10.4274/tjps.galenos.2021.33733
[12] Moussa BA. Determination of some aminobenzoic acid derivatives: glafenine and metoclopramide. Journal of Pharmaceutical and Biomedical Analysis. 2000;23(6):1045-55. https://doi.org/10.1016/S0731-7085(00)00384-8 DOI: https://doi.org/10.1016/S0731-7085(00)00384-8
[13] Patel SA, Patel CN, Patel MM. Visible spectrophotometric methods for the estimation of metoclopramide hydrochloride in tablets. Indian Journal of Pharmaceutical Sciences. 2006;68(3):397-9. DOI: https://doi.org/10.4103/0250-474X.26663
[14] Al-Azzawi HAW, Al-Obadi FM, Al-Sabha, TN. Spectrophotometric assay of metoclopramide hydrochloride in bulk and in dosage form. Iraqi National Journal of Chemistry. 2015;15(1):59-76.
[15] Devi OZ, Basavaiah K, Vinay KB, Revanasiddappa HD. Sensitive spectrophotometric determination of metoclopramide hydrochloride in dosage forms and spiked human urine using vanillin. Arabian Journal of Chemistry. 2016;9:S64-S72. https://doi.org/10.1016/j.arabjc.2011.02.017 DOI: https://doi.org/10.1016/j.arabjc.2011.02.017
[16] Naggar AH, Elnasr TAS, Sayed Ali AS, Kotb A, El Sayed AAY. Determination of metoclopramide hydrochloride in pharmaceutical formulations using three different spectrophotometric methods. Pharmaceutica Analytica Acta. 2017;8(2):1000538. https://doi.org/10.4172/2153-2435.1000538 DOI: https://doi.org/10.4172/2153-2435.1000538
[17] Ali R, Othman N. Spectrophotometric determination of metoclopramide hydrochloride in pharmaceutical preparations via Schiff’s base reaction. In: Advances in Health Sciences Research, vol. 38: Proceedings of the 1st International Ninevah Conference on Medical Sciences (INCMS 2021). Atlantis Press; 2021. p. 63-69. https://doi.org/10.2991/ahsr.k.211012.011 DOI: https://doi.org/10.2991/ahsr.k.211012.011
[18] Thanoon ES, Saeed AMA. Development of green spectrophotometric method for determination of metoclopramide hydrochloride. Egyptian Journal of Chemistry. 2021;64(7):3451-6.
[19] Shah J, Jan MR, Khan MA, Amin S. Spectrophotometric determination of metoclopramide in pharmaceutical preparations. Journal of Analytical Chemistry. 2005;60(7):633-35. https://doi.org/10.1007/s10809-005-0151-5 DOI: https://doi.org/10.1007/s10809-005-0151-5
[20] Mahmood HS, Shaker ZT, Taha L. Spectrophotometric assay of metoclopramide in pharmaceutical preparations. Tikrit Journal of Pharmaceutical Sciences. 2007;3(1):1-5. https://doi.org/10.25130/tjphs.2007.1.1.1.5 DOI: https://doi.org/10.25130/tjphs.2007.1.1.1.5
[21] Sinan R, Abed SS. Spectrophotometric determination of metoclopramide hydrochloride in tablets by diazotization and coupling reaction with phenol. Iraqi Journal of Science. 2009;50(2):136-43. https://doi.org/10.24996/ijs.2009.50.2.%25g
[22] Sultan SH. Spectrophotometric determination of metoclopramide hydrochloride in pharmaceutical preparations by the diazotization-coupling method with phloroglucinol. Tikrit Journal of Pure Science. 2009;14(1):155-60.
[23] Sinan R. Spectrophotometric determination of metoclopramide hydrochloride in pharmaceutical tablets, by diazotization-coupling method with 1-naphthol as the coupling agent. Baghdad Science Journal. 2010;7(1):704-12. https://doi.org/10.21123/bsj.2010.7.1.704-712 DOI: https://doi.org/10.21123/bsj.7.1.704-712
[24] Sarsam LA, Mohammed SA, Al-Abbasi KM. Spectrophotometric determination of metoclopramide hydrochloride in pharmaceutical preparations using diazotization reaction. Rafidain Journal of Science. 2011;22(3):76-88. https://doi.org/10.33899/rjs.2011.6509 DOI: https://doi.org/10.33899/rjs.2011.6509
[25] Devi OZ, Basavaiah K, Vinay KB, Revanasiddappa HD. Determination of metoclopramide hydrochloride in pharmaceuticals and spiked human urine through diazotization reaction. Journal of Food and Drug Analysis. 2012;20(2):454-63. https://doi.org/10.6227/jfda.2012200204
[26] Jawad AA, Kadhim KH. Spectrophotometric determination of metoclopramide hydrochloride in bulk and pharmaceutical preparations by diazotization-coupling reaction. International Journal of Pharmacy and Pharmaceutical Sciences. 2013;5(Suppl. 3):294-98.
[27] Obedagha AN, Aljarah RN. Development of spectrophotometric method for the determination of metoclopramide HCl in a pharmaceutical preparations. Rafidain Journal of Science. 2014;25(2):10-21. https://doi.org/10.33899/rjs.2014.88564 DOI: https://doi.org/10.33899/rjs.2014.88564
[28] Pratapareddy AJ. New spectrophotometric determination of metoclopramide in bulk and pharmaceutical dosage form. Journal of Drug Discovery and Therapeutics. 2015;3(35):01-04.
[29] Taha HKA, Al-Rufaie MM, Motaweq ZY. Spectrophotometric determination of metoclopramide medicine in bulk form and in pharmaceuticals using orcinol as reagent. Ovidius University Annals of Chemistry. 2018;29(2):85-91. https://doi.org/10.2478/auoc-2018-0012 DOI: https://doi.org/10.2478/auoc-2018-0012
[30] Abbas SM, Jamur JMS, Nasif AM. Spectrophotometric method for the determination of metoclopramide in pharmaceutical forms. Journal of Applied Spectroscopy. 2021;88(2):433-40. https://doi.org/10.1007/s10812-021-01191-7 DOI: https://doi.org/10.1007/s10812-021-01191-7
[31] Ganduh SH, Aljeboree AM, Mahdi MA, Jasim LS. Spectrophotometric determination of metoclopramide-HCl in the standard raw and it compared with pharmaceuticals. Journal of Pharmaceutical Negative Results. 2021;12(2):44-8.
[32] Mubder NS, Kadhim EA, Ibraheem IH, Mahmood H, Dhahir SA, Al-Neshmi H. Micro spectrophotometric determination and cloud point extraction of metoclopramide with 4-nitro phenol in pure form and pharmaceutical drugs. Annals of the Romanian Society for Cell Biology. 2021;25(4):12088-103.
[33] Alhammadi GA, Sarsam LA. Novel green method for the spectrophotometric determination of metoclopramide hydrochloride in pharmaceutical formulations. Journal of the Turkish Chemical Society Section A: Chemistry. 2023;10(1):193-204. https://doi.org/10.18596/jotcsa.1158403 DOI: https://doi.org/10.18596/jotcsa.1158403
[34] Yassin RMA, Othman NS. Spectrophotometric determination of metoclopramide hydrochloride in pharmaceutical formulations using diazotization coupling reaction. Iraqi Journal of Science. 2023;64(9):4312-28. https://doi.org/10.24996/ijs.2023.64.9.1 DOI: https://doi.org/10.24996/ijs.2023.64.9.1
[35] Ahmad NR, Ali NM. Spectrophotometric determination of metoclopramide in some pharmaceutical preparations via oxidative coupling reaction. Journal of Education and Science. 2006;18(4):16-22. DOI: https://doi.org/10.33899/edusj.2006.77240
[36] Delfino MR, Monzón CM, Hernández SR, Sarno MDC. Metoclopramide–nitrite reaction. Validation of its application to the spectrophotometric analysis of generic tablets. IOSR Journal of Pharmacy. 2012;2(5):27-34. https://doi.org/10.9790/3013-25702734 DOI: https://doi.org/10.9790/3013-25702734
[37] Salih ES, Mohamad IK, Al-Najafi SI. Spectrophotometric assay of metoclopramide hydrochloride in pharmaceutical preparations via oxidative coupling reaction with promazine hydrochloride and N-Bromosuccinimide. Journal of Education and Science. 2006;18(3):10-9. DOI: https://doi.org/10.33899/edusj.2006.162867
[38] Othman NS, Mahmood HS, Khaleel NA. Spectrophotometric determination of metoclopramide hydrochloride in pharmaceutical preparations via oxidative coupling reaction. Tikrit Journal of Pure Science. 2011;16(4):89-95.
[39] Al-Shaker YM. Spectrophotometric assay of metoclopramide hydrochloride in some pharmaceutical preparations via oxidation coupling reaction. Iraqi Journal of Pharmacy. 2013;13(1):41-50. DOI: https://doi.org/10.33899/iphr.2013.066898
[40] Yassin RMA, Othman NS. Using of oxidative-coupling reaction in spectrophotometric determination of metoclopramide hydrochloride in pharmaceutical preparations. Basrah Journal of Sciences. 2022;40(2):465-85. https://doi.org/10.29072/basjs.20220215 DOI: https://doi.org/10.29072/basjs.20220215
[41] Devi OZ, Basavaiah K, Vinay KB. Application of potassium permanganate to spectrophotometric assay of metoclopramide hydrochloride in pharmaceuticals. Journal of Applied Spectroscopy. 2012;78(6):873-83. https://doi.org/10.1007/s10812-012-9547-9 DOI: https://doi.org/10.1007/s10812-012-9547-9
[42] Shekho NH, Al-Sarraj TZ. Spectrophotometric assay of metoclopramide hydrochloride in pharmaceutical preparations via arsenazo III-cerium (III) reaction. Rafidain Journal of Science. 2013;24(1):70-83. https://doi.org/10.33899/rjs.2013.67502 DOI: https://doi.org/10.33899/rjs.2013.67502
[43] Abdulkareem HM, Al-Tameemi M, Ibraheem IH, Hadi MS. Surfactant cloud point extraction as a procedure of preconcentrating for metoclopramide determination using spectroanalytical technique. Baghdad Science Journal. 2020;17(1):57-65. https://doi.org/10.21123/bsj.2020.17.1.0057 DOI: https://doi.org/10.21123/bsj.2020.17.1.0057
[44] Ahmed NR, Saadallah NC, Ahmed AI. Estimation of metoclopramide HCl in pharmaceutical preparations and environmental water samples. World Journal of Pharmacy and Pharmaceutical Sciences. 2020;9(1):151-59. https://doi.org/10.20959/wjpps20201-15283
[45] International Conference on Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human Use. Validation of analytical procedures: text and methodology Q2(R1). London: International Conference on Harmonization; 2005.
[46] Amin MM, El-Adl SM, Abdel-Aziz SA, Mostafa SM. Bromometric estimation of gliclazide and glibenclamide in bulk and in tablet formulation. Zagazig Journal of Pharmaceutical Sciences. 2015;24(2):97-108. https://doi.org/10.21608/zjps.2015.38167 DOI: https://doi.org/10.21608/zjps.2015.38167
[47] British Pharmacopoeia. The British Pharmacopoeia, London: The Stationery Office on behalf of the Medicines and Healthcare products Regulatory Agency; 2020.
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