In this study, we propose an easy approach by combining the Fourier transform infrared and attenuated total reflectance (FTIR-ATR) spectroscopy together with chemometrics analysis for rapid detection and accurate quantification of five adulterants such as fructose, glucose, sucrose, corn syrup and cane sugar in stingless bees (Heterotrigona itama) honey harvested in Malaysia. Adulterants were classified using principal component analysis and soft independent modeling class analogy, where the first derivative of the spectra in the wavenumber range of 1180-750cm-1 was utilized. The protocol could satisfactorily discriminate the stingless bees honey samples that were adulterated with the concentrations of corn syrup above 8% (w/w) and cane sugar over 2% (w/w). Feasibility of integrating FTIR-ATR with chemometrics for precise quantification of the five adulterants was affirmed using partial least square regression (PLSR) analysis. The study found that optimal PLSR analysis achieved standard error of calibrations and standard error of predictions within an acceptable range of 0.686-1.087% and 0.581-1.489%, respectively, indicating good predictive capability. Hence, the method developed here for detecting and quantifying adulteration in H. itama honey samples is accurate and rapid, requiring only 7-8min to complete as compared to 3h for the standard method, AOAC method 998.12.
We report an efficient sample preparation method (freezing) for onsite fat and meat analysis via a specially designed thermoelectric cooling and temperature-controlling system. This investigation also focused on the effect of phase change on the sensitivity and reproducibility of LIBS emission signals and plasma parameters. The plasma emissions of animal fats (lard) were recorded when the sample was frozen (-2 °C), fluid (15 °C), and in a liquid state (37 °C) with a thermoelectric cooling system. At each temperature, the plasma emissions were acquired at laser pulse energy from 50 to 300 mJ and detector gate delay (DGD) from 0.5 to 5 μs. With increasing sample temperature, the DGD, where the optical emission intensity reached a maximum, decreased. At a laser pulse energy of 200 mJ and a sample temperature of -2 °C, the emission signals increased fourfold, the signal-to-noise ratio (SNR) improved tenfold, and the self-absorption in the emission lines decreased significantly. The repeatability of the emission signals and plasma parameters of frozen and liquid fat samples was determined using the relative standard deviation (RSD) of Se I (473.08 nm) and K I (766.48 nm) emission lines. The RSDs of the emission signals improved from 40 to 18 % and 37 to 16 %, whereas the shot-to-shot RSDs of the electron temperature and electron number density get improved from 11 to 6 % and 12 to 6.8 %, respectively.