Detection of meloxicam residues in milk using ATR- FTIR spectroscopy coupled with chemometrics

Abstract

Meloxicam (MELX), a non-steroidal anti-inflammatory drug (NSAID), is frequently administered to cattle, poses a risk to human health when it is found in milk. Regulatory bodies of EU, Canada, China and India have prescribed maximum residue limits for MELX in milk as 15, 35 and 15 and 10 μg/kg, respectively. This study explores the use of attenuated total reflectance- Fourier transform infrared (ATR-FTIR) spectroscopy in conjunction with chemometric techniques to detect MELX residues in milk. Samples of pure milk and milk samples spiked with MELX at different concentrations ranging from 1 to 50 μg/kg were analysed. ATR-FTIR measurements were taken in the wavenumber range of 4000–400 cm−1 for all the samples. Principal component analysis (PCA) was applied in the regions of 2940–2840 and 1765–1730 cm−1 to differentiate clusters of milk sample with those of MELX and milk spiked with MELX samples. The coefficient of determination (R2) values for calibration and validation sets in wavenumber regions of 2940–2840 and 1765–1730 cm−1 were >0.92 and > 0.94, respectively for the developed partial least squares regression (PLSR) models. All the samples showed 100% classification efficiency using the soft independent modeling of class analogy (SIMCA) technique. The study concluded that the presence of MELX residues can be detected in milk even at 1 μg/kg level using ATR-FTIR and chemometrics. Results obtained from developed FTIR based chemometric method were in agreement with those obtained from LC-MS/MS method and have the potential for application in screening milk samples for the presence of MELX.