In this study, a multi-residue analysis was developed for 32 compounds, including pesticides and metabolites, in five meat products using gas chromatography-tandem mass spectrometry (GC-MS/MS). The validation of the developed analytical method was also evaluated in accordance with Codex Alimentarius guidelines. Aminopropyl (NH2), C18, and florisil solid phase extraction (SPE) cartridges were used to evaluate and optimize the cleanup procedure of the tested samples prior to GC-MS/MS analysis. Based on the analytical performance, the C18 SPE cartridge was deemed to be the most suitable among the examined SPE cartridges. The optimized method demonstrated that 29 out of 32 tested compounds acquired good linearity (R2 ≥ 0.99), and 25 tested compounds displayed the method limit of quantification (MLOQ) ≤ 0.01 mg/kg. Out of the 32 tested compounds, only 21 compounds met the acceptable analytical criteria for the lard and tallow samples, compared to 27 compounds in the beef, pork, and chicken samples that falls within the acceptable standards for recovery (70–120%) and analytical precision (relative standard deviation RSD ≤ 20%). The average matrix effect was widely varied (20.1–64.8%) in the studied meat samples that were affected by either ion enhancement or suppression. In particular, in the lard sample, 13 compounds showed poor recovery and analytical precision due to ion suppression. Thus, the matrix effect (ME) was considered a critical factor during multi-residue pesticide analysis in different meat products. In conclusion, this developed analytical method can be used as a routine monitoring system for residual pesticide analysis in livestock products with acceptable analytical standards. Further meticulous analytical studies should be optimized and validated for multi-residue pesticide analysis in diversified meat products.
31 December 2019 in Journal of Applied Biological Chemistry
We report the effects of excess Si phase on the C54 transformation and the thermal stability of TiSi2 thin films as a function of Si/Ti (x) ratio. The resistivity and x-ray diffraction data of TiSix(x=2.1–2.4) films showed a retardation of C54–TiSi2 transformation with incremental molar ratio x; the TiSix (x=2.1–2.3) films were completely transformed to C54-TiSi2 with rapid thermal annealing (RTA) of 750 °C, while the TiSix (x=2.4) films were transmuted to C54–TiSi2 over the RTA of 800 °C. Transmission electron microscopy study revealed that the growth of Si precipitates in the Si-rich TiSix films competes with the grain growth during the transformation of C49 to C54 TiSi2 phase, resulting in the increase of C54 transformation temperature. An excellent sheet resistance (Rs) and its standard deviation in concert with a reliable gate oxide integrity were attained from the Si-rich TiSi2/polycrystalline-Si (poly-Si) structure up to the solid state annealing of 850 °C for 60 min. These attributes are due to the reduced solid state reaction at TiSi2/Si interface and the suppressed TiSi2 agglomeration by Si precipitates. The average Rs of the 0.12-μm-wide TiSi2(800 Å)/poly-Si gate lines is lower than 4.5 Ω/□, demonstrating a robust gate electrode structure for gigabit scale device application.
31 March 2025 in The Korean Journal of Pesticide Science