| Acrylamide, in foodstuffs, causes considerable concern as AM has been known to be a neurotoxic, genotoxic and carcinogenic compound. Acrylamide pollution in food is becoming a hot spot of research. For controlling the acrylamide pollution effectively, to develop an accurate and reliable analytical method is highly required.This study prepares two kinds of novel materials which have the higher adsorption in toward acerylamide. They have been used as the adsorption of solid-phase extraction and matrix solid-phase dispersion extraction, respectively. Both of them coupled with high-performance liquid chromatograph, and two novel methods for determination of trace acrylamide in food were developed.SPE-HPLC method for the determination of trace acrylamide in foodstuffs.In this study, a novel functionalized material was synthesized by immobilized the ionic liquid onto the activated silica gel surface using the glutaraldehyde(1%, m/m) as the cross-linker. The adsorption ability of the prepared material toward acrylamide was evaluated by static adsorption experiments, and the results showed that it had high adsorption capacity. Scatchard analysis indicated that the binding sites in the prepared material had two distinct groups. The saturated adsorption capacity(Qmax1) was 7.9 mg g-1 due to the high affinity binding sites, and another saturated adsorption capacity(Qmax2) was 2.3 mg g-1 due to the low affinity binding sites. This prepared material also offered fast kinetics for adsorption of the acrylamide. After shaking for 30 min, 60.0% of the equilibrated adsorption capacity was obtained, and the adsorption almost reached equilibrium within 180 min.This material was applied as sorbent, and a method of solid-phase extraction coupled with high-performance liquid chromatography(SPE-HPLC) for analysis of acrylamide in foods was developed. Under optimal conditions, the limit of detection(S/N = 3) of this method for acrylamide was 4.2 μg L-1, and the RSD for five replicate extractions of 50 μg L-1 acrylamide was 4.5%. The blank potato and bread crumb samples spiked with acrylamide at different levels of 1.0 and 10.0 μg g-1 were extracted and determined respectively by this developed method, and recoveries ranging from 86.3% to 90.3% were obtained. Finally, this method was applied to quantitative detection of acrylamide in bread crust and cracker samples.MSPD-HPLC method for the determination of trace acrylamide in foodstuffs.In this research, the chitosan grafted multi-walled carbon nanotubes(CS/MWCNT-OX) were synthesized and characterized by the Fourier-transform infrared(FT-IR), transmission electron microscope(TEM), X-ray diffraction(XRD), thermogravimetric analysis(TGA), static and kinetic adsorption experiments. Results showed the resulting material had good adsorption ability and rapid dynamic towards acrylamide.Using this material as sorbent, a method of matrix solid phase dispersion extraction(MSPD) coupled with high-performance liquid chromatography(MSPD-HPLC) for determination of trace acrylamide in foods was developed. Under optimal conditions, the limit of detection(LOD) based on three times the signal-to-noise ration of the baseline near the analyte peak was 1.5 μg L-1, the RSD for five replicate extractions of 50 μg L-1 acrylamide was 4.3%. The blank potato and flour samples spiked with acrylamide at different levels of 2.25, 4.50 and 6.75 μg kg-1 were extracted and determined by this developed method with good recoveries ranging from 85.3% to 94.6%. This method was used for quantitative analysis of acrylamide in different food samples including twisted cruller, potato chip and toast samples. Compared to other methods, this developed method was demonstrated to be rapid and simple for extraction and determination of trace acrylamide in food samples. |
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