A non-destructive NIR spectroscopic method combined with chemometry for simultaneous assay of paracetamol and caffeine in tablets

• Published in: Practica farmaceutică (Online) Vol. 57; no. 2; pp. 68 - 75
• Main Authors: MUNTEAN, Dana, PORFIRE, Alina, ALECU, Cristian, IURIAN, Sonia, CASIAN, Tibor, GÂVAN, Alexandru, TOMUTA, Ioan
• Format: Journal Article
• Language: English
• Published: Amaltea Medical Publishing House 30.06.2021
• Subjects: api assay; caffeine; chemometry; nir spectroscopy; paracetamol; tablets
• ISSN: 2066-5563; 2069-6671
• DOI: 10.37897/RJPhP.2021.2.2

The use of near infrared (NIR) spectroscopy to predict the concentration of two active pharmaceutical ingredients (APIs), paracetamol and caffeine, in intact tablets, has been evaluated in this study. A partial least squares (PLS) regression model was developed using spectral data obtained on a calibration set consisting of 28 formulations containing 80, 90, 100, 110 and 120% of each API. Regression models were developed for each API, both using un-processed spectral data as well as after applying various spectra pre-processing methods. Cross-validation was used to select best calibration model. The selected model was validated in terms of precision, trueness, accuracy and linearity in a concentration ranging from 90 to 110% of the targeted APIs concentration. The applicability of the method was tested on tablets containing 300 mg paracetamol and 30 mg caffeine as targeted composition, and the API content predicted by the proposed NIR-chemometric method was not statistically different from the one obtained by HPLC method, used as a reference method. Thus, the method presented in the current paper is a step forward towards the implementation NIR as useful tool for monitoring the manufacturing process of fixed-dose combination tablets with paracetamol and caffeine.