Quantitative determination algorithm of acetylsalicylic acid by FTIR spectrometr

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Abstract

Introduction. The article presents an algorithm for the quantitative determination of acetylsalicylic acid by Fourier-transform infrared (FTIR) spectroscopy in the mode of disturbed total internal reflection on the example of the analysis of mixtures similar to the composition of tablet dosage form. The study aims to develop an algorithm and a mathematical model based on the partial least squares (PLS) method. The proposed algorithm allows to exclude the stage of dissolution of samples, reduce the analysis time and can be adapted for the quantitative determination of other organic substances in solid dosage forms.

Objective. Development and approbation of an algorithm for the quantitative determination of acetylsalicylic acid in solid multicomponent mixtures using FTIR-spectrometry with a mathematical model based on the partial least squares method.

Material and Methods. The study was carried out on a model mixture of tablet mass, similar of tablets “Acetylsalicylic acid” 500 mg (OJSC “Dalchimpharm”). 30 calibration and 15 control samples were prepared by mixing acetylsalicylic acid substance with a mixture of excipients. IR spectra were recorded on a Cary 630 FTIR spectrometer (Agilent, USA) in the range of 4000-650 cm-¹ (resolution: 4 cm-¹). Data were processed in KNIME 4.5.7 using the Python 3.9.10 package and the scikit-learn 1.3.0 library. Processing stages: normalization, multiplicative scattering correction, separation of spectrometric data into training/test sets (in the ratio 70:30 according to the Kennard-Stone method), obtaining a calibration (“mathematical”) model by the PLS method, testing the predictive ability of the model on the test set, and testing the model on control samples of acetylsalicylic acid.

Results. The determination coefficient (r²) of the mathematical model when analyzing the test sample of spectrometric data was 0.97, which confirms its high predictive ability. When tested on control samples of acetylsalicylic acid, the relative deviation of the calculated concentration from the actual one did not exceed ±5%.

Conclusions. An algorithm for the quantitative determination of acetylsalicylic acid by infrared spectrometry in the mode of disturbed total internal reflection based on the partial least squares method was developed and tested. The relative deviation of ±5% in a wide range of concentrations indicates the applicability of the algorithm for the development of a technique for the quantitative analysis of acetylsalicylic acid by FTIR-spectrometry. Further optimization of spectrometric data processing in order to increase the predictive ability of mathematical models will allow to implement the algorithm in quality control of tablet dosage forms.

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About the authors

A. V. Voronin

Samara State Medical University of the Ministry of Healthcare of the Russian Federation

Author for correspondence.
Email: a.v.voronin@samsmu.ru
ORCID iD: 0000-0002-8472-3796
SPIN-code: 5727-4822

Dr.Sc. (Pharm.), Institute of Pharmacy, Professor, Head of the Department of Chemistry

Russian Federation, 89 Chapaevskaya Street, Samara, 443099

D. N. Markin

Samara State Medical University of the Ministry of Healthcare of the Russian Federation

Email: d.n.markin@samsmu.ru
ORCID iD: 0009-0001-6376-6818
SPIN-code: 1565-9663

Institute of Pharmacy, Post-graduate Student, Department of Chemistry

Russian Federation, 89 Chapaevskaya Street, Samara, 443099

A. V. Karpov

Samara State Medical University of the Ministry of Healthcare of the Russian Federation

Email: al.v.karpov@samsmu.ru
ORCID iD: 0000-0002-0780-0241
SPIN-code: 5606-3506

Ph.D. (Pharm.), Institute of Pharmacy, Assistant, Department of Chemistry

Russian Federation, 89 Chapaevskaya Street, Samara, 443099

D. A. Zhdanov

Samara State Medical University of the Ministry of Healthcare of the Russian Federation

Email: d.a.zhdanov@samsmu.ru
ORCID iD: 0000-0002-8285-6296
SPIN-code: 1629-5490

Ph.D. (Pharm.), Institute of Pharmacy, Senior Lecturer, Department of Chemistry

Russian Federation, 89 Chapaevskaya Street, Samara, 443099

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2. Fig. 1. IR spectra of samples: A – acetylsalicylic acid reference materiala (acetylsalicylic acid concentration 100.0% (wt.)); Б – «Acetylsalicylic Acid», 500 mg tablet; В – excipient mixtures (acetylsalicylic acid concentration 0% (wt.))

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3. Fig. 2. Testing the predictive ability of a mathematical model for the quantitative determination of acetylsalicylic acid in mixtures similar to the composition of “Acetylsalicylic acid” 500 mg tablets

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4. Fig. 3. Algorithm for the quantitative determination of acetylsalicylic acid in mixtures similar to the composition of «Acetylsalicylic acid» 500 mg tablets by FTIR

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