In this study, a simple solid-phase extraction (SPE) approach by using activated attapulgite as sorbent was successfully developed for the determination of melamine in milk formula samples. Crucial factors impacting the extraction efficiency, including sample solvent, elution solvent, and sample loading volume, were investigated. Under the optimal extraction conditions, the sample loading volume was up to 200 mL and the adsorption capacity of the melamine gave rise to 1154 μg g(-1). Excellent linear calibration curves (r (2) > 0.999) were achieved, and then the limit of detection (S/N = 3) and the limit of quantification (S/N = 10) were found to be 0.15 and 0.5 ng mL(-1), respectively. The recoveries of the melamine spiked in four milk formula samples at three concentration levels ranged from 83.5 to 111.0 % with relative standard deviations (RSDs) less than 10.2 %. Furthermore, RSDs of batch to batch (n = 4) of the acidified attapulgite used in this developed method were in the range of 2.3∼7.3 %. In comparison to the commercial Oasis MCX, the acidified attapulgite sorbent even outperformed (at least in terms of reproducibility) for melamine analysis in real food samples. Because of its simplicity, the newly developed SPE method based on acidified attapulgite nanoparticles should provide a promising tool for daily monitoring of doped melamine in milk formula or other complex matrices.
In this work, the effect of solvent pre-treatment (hexane, petroleum ether and ethanol) on the physicochemical, thermal and morphology behavior of
Mangifera pajang
seed fat (MPSF) were investigated. Fat extraction was performed using Soxhlet method, and results showed that the yield, physicochemical, and crystalline structures of the MPSF were significantly (p < 0.05) influenced by the extraction solvents. Hexane gave the highest fat yield (7.67 %) with low unsaturation value (52.13 g iodine/g) compared with petroleum ether and ethanol. Hexane MPSF also had low oxidation rate (peroxide value of 1.1 mEq/g). Both non-stabilized and stabilized hexane MPSF showed a single melting endothermic peak at high temperature with onset, maximum peak and offset temperature of 16.23 ˚C-18.21 °C, 28.22 ˚C-31.25 °C and 34.85 ˚C-39.58 °C, respectively. Hexane MPSF crystallized rapidly at high temperature with single maximum peak starting at 16.51 ˚C-16.68 °C and ending at 0.23 ˚C-1.13 °C. In comparison with ethanol extract, hexane MPSF demonstrated a compact crystalline structure with a large densely packed center. Therefore, MPSF obtained from hexane presented better overall quality than those obtained from other extraction solvents. MPSF exhibited similar melting and morphological behavior to mango kernel fat and commercial cocoa butter. These results suggested that hexane was the best solvent for the extraction of MPSF. This fat also has the potential to be applied as a cocoa butter alternative fat or functional fat.
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