RAPID ATTENUATED TOTAL REFLECTANCE–FOURIER TRANSFORM INFRARED SPECTROSCOPIC QUANTIFICATION OF ATENOLOL IN ITS MICROSPHERES AND TABLETS: A GREEN APPROACH
DOI:
https://doi.org/10.22159/ajpcr.2026v19i4.58212Keywords:
Atenolol, ATR- FTIR, Quantification, Validation, AnalysisAbstract
Objective: A solvent-free direct quantification of atenolol (ATN)-loaded microspheres and its tablets by utilizing attenuated total reflectance (ATR)– Fourier transform infrared (FTIR) spectroscopy was the prime objective of the current research work.
Methods: Developing a non-destructive analytical method to quantify the polymer-based analyte is a tremendous task. Since there is a lacuna in the analysis of drugs in the presence of interfering formulation excipients, we proposed an ATR-FTIR spectroscopic method for the qualitative and quantitative estimation of ATN in its polymer-based microsphere formulations. This ATR-FTIR spectroscopic analysis is based on the measurement of the absorption bands and deriving the linearity calibration curve for the effective quantification of ATN in its formulations.
Results and Discussion: The prominent absorption was found at 1235 cm⁻1 due to the stretching of the C-O-C aromatic ether linkage moiety of ATN. The linearity of absorbance versus the concentration was found in the range 10–100%w/w with the r2=0.9960. The high percentage of recovery of ATN in microspheres and its marketed tablets (99.76 and 99.66% w/w) demonstrates the compliance of the accuracy study limits as per the International Council for Harmonisation guidelines. Precision study results showed acceptable % relative standard deviation values. The limit of detection and limit of quantification values (0.7 % w/w and 2.0 % w/w, respectively) indicated the high sensitivity of the method. The polymer excipients of the ATN-loaded microsphere and in the commercial tablet preparation did not interfere with the active drug.
Conclusion: Thus, the developed ATR-FTIR spectroscopic method is non-destructive, solvent-free, green, inexpensive, accurate, and rapid technique for quantitative determination of ATN in their polymer microspheres and tablet formulations.
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References
1. Sweetman SC. Martindale. London: Pharmaceutical Press; 2005. p. 865, 933, 47.
2. O’Neil MJ, Heckelman PE, Koch CB, Roman KJ, editos, The merck index - An encyclopedia of chemicals, drugs, and biologicals. 14ed. Whitehouse Station, NJ: The Merck Index, Merck and Co., Inc.; 2001. p. 147.
3. Ministry of Health and Family Welfare. Indian Pharmacopoeia, Controller of Publications. Vol. 4. New Delhi: Ministry of Health and Family Welfare, Government of India; 1996. p. 72-5.
4. Annapoorani A, Ruby S, Kumar M. Eco-friendly quantitative assessment of amlodipine besylate in its microspheres and commercial tablets using ATR-FTIR spectroscopy. Int J Drug Deliv Technol. 2025;15(3):1094-100.
5. Bansal R, Guleria A, Acharya PC. FT-IR method development and validation for quantitative estimation of zidovudine in bulk and tablet dosage form. Asian J Pharm Sci. 2011;4(3):306-13.
6. Konoz E, Sarrafi AH, Samadizadeh M, Boreiri S. Quantitative analysis of lorazepam in pharmaceutical formulation through FTIR spectroscopy. E-J Chem. 2012;9(2232):2238.
7. Bhoomendra B, Sirajunisa T, Sunil DA. Validated method for the quantitation of ciprofloxacin hydrochloride using diffuse reflectance infrared Fourier transform spectroscopy. Int J Spectrosc. 2014;12:1-6.
8. Patraa KC, Kumarb KJ, Sahooa SK, Suresha P. Rapid FTIR method for estimation of sucrose in a traditional Indian polyherbal formulation. Euras J Anal Chem. 2010;5:73-80.
9. Mazarevica G, Diewok J, Baena JR, Rosenberg E, Lendl B. On-line fermentation monitoring by mid-infrared spectroscopy. Appl Spectrosc. 2004;58(7):804-10.
10. Matkovic SR, Valle GV, Briand LE. Quantitative analysis of ibuprofen in pharmaceutical formulations through FTIR spectroscopy. Lat Am Appl Res. 2005;25:189-95.
11. Yilmaz B, Arslan S, Asci A. HPLC method for determination of atenolol in human plasma and application to a pharmacokinetic study in Turkey. J Chromatogr Sci. 2012;50(10):914-9. doi: 10.1093/chromsci/bms090, PMID 22718748
12. Kumar N, Verma N, Songh O, Joshi N, Singh KG. Estimation of atenolol by reverse phase high performance liquid chromatography. E J Chem. 2010;7(3):962-6.
13. El-Alfy W, Ismaiel OA, El-Mammli MY, Shalaby A. Determination of atenolol and trimetazidine in pharmaceutical tablets and human urine using a high performance liquid chromatography-photo diode array detection method. Int J Anal Chem. 2019;2019:9625849. doi: 10.1155/2019/9625849, PMID 30719043
14. Elkady EF, Fouad MA, Faquih AA. A versatile stability-indicating liquid chromatographic method for the simultaneous determination of atenolol, hydrochlorothiazide and chlorthalidone. Curr Pharm Anal. 2020;16(8):1037-51. doi: 10.2174/1573412915666190523122525
15. Madhusudhan P, Reddy KV, Singh SA. Novel isocratic RP-HPLC method development and validation for simultaneous determination of atenolol and nifedipine in tablet dosage form. Univers Rev. 2018;7(9):412-21.
16. Peleshok K, Piponski M, Kovalenko S, Ahmed H, Abdel-Megied A, Ezike OF. New liquid chromatography assays for simultaneous quantification of antihypertensives atenolol and valsartan in their dosage forms. J Sep Sci. 2021;44(2):565-75. doi: 10.1002/jssc.202000859, PMID 33226168
17. El-Gindy A, Emara S, Mostafa A. HPLC and chemometric-assisted spectrophotometric methods for simultaneous determination of atenolol, amiloride hydrochloride and chlorthalidone. Farmaco. 2005;60(3):269-78. doi: 10.1016/j.farmac.2004.11.013, PMID 15784248
18. Goebel K, Rolim CM. Validation of UV spectrophotometric and HPLC methods for quantitative determination of atenolol in pharmaceutical preparations. Lat Am J Pharm. 2007;26(5):760-5.
19. Vaikosen EN, Bioghele J, Worlu RC, Ebeshi BU. Spectroscopic determination of two beta blockers-atenolol and propanolol by oxidative derivatization using potassium permanganate in alkaline medium. Rev Anal Chem. 2020;39(1):56-64. doi: 10.1515/revac-2020-0103
20. Kori S, Goyal J, Sharma S, Pahade NK, Tandekar M. Method development and validation of atenolol drug by spectrophotometric and HPLC technique in forensic application. Int J Sci Res. 2013;4:438.
21. Al-Awadie NS, Khudhair AF. Determination of Atenolol in pharmaceutical formulations by continuous flow injection analysis via turbidimetric (T180o) and scattered light effect at two opposite position (2N90o) using Ayah 4SW-3D-T180-2N90- Solar-CFI analyser. Iraqi J Sci. 2014;55(1):12-26.
22. Madhurai P, Babu GR, Rao PS, Kiran BS, Kumari MV. Quantitative estimation of atenolol in pharmaceutical dosage forms by using visible spectroscopy. Int J Pharm Chem Biol Sci. 2015;5(3):557-60.
23. Annapoorani A, Ruby S, Kumar M, Bhuvaneswari R. Simple, rapid, and a green derivative ATR-FTIR spectroscopic method for the analysis of atenolol loaded microspheres and its tablet formulations. Biol Forum Int J. 2023;15(5):1051-7.
24. Fiveable. 18.8 Spectroscopy of Ethers. United States: Fiveable; 2024 May 7.
25. Almirall J. Quantitative analysis in drug formulations: methods, challenges, and innovations. Pharm Anal Chem. 2024;9:234.
26. Das S, Mandal S, Mandal S, Saha S. Design, development, and evaluation of vildagliptin-loaded crosslinked sodium alginate and Moringa gum microspheres by ionotropic gelation method and in silico study using pk-sim software. Asian J Pharm Clin Res. 2026;19(2):97-107.
27. Al-Tahami K. Preparation, characterization, and in vitro release of ketoprofen loaded alginate microspheres. Int J Appl Pharm. 2014;6(3):9-12.
28. Nayak AK, Pal D, Pradhan J, Hasnain MS. Fenugreek seed mucilage-alginate mucoadhesive beads of metformin HCl: Design, optimization and evaluation. Int J Biol Macromol. 2013;54:144-54. doi: 10.1016/j. ijbiomac.2012.12.008, PMID 23246901
29. Dey P, Sa B, Maiti S. Impact of gelation period on modified locust bean-alginate interpenetrating beads for glipizide delivery. Int J Macromol. 2015;76:176-80.
30. ICH. Q2A. Guidelines on validation of analytical procedure: Definitions and terminology. Fed Regist. 1995;60:11260.
31. ICH. Q2B. Guidelines on validation of analytical procedure: Methodology. Fed Regist. 1996;60:27464.
32. Indrani B, Ghosh SK. Development and validation of stability indicating RP-HPLC method for the determination of atenolol and hydrochlorthiazide in combined solid dosage form. Int J Pharm Pharm Sci. 2015;7(2):489-92.
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