Pesticides and polychlorinated biphenyls (PCBs) are found in various parts of the environment in quite small concentrations, but they accumulate and thus become a threat to human health and life. A review is focused on the application of some popular techniques for sample preparation in analysis of these compounds in food. Even with the emergence of advanced techniques of final analysis, complex matrices, such as food, require extensive sample extraction and purification. Traditional sample preparation techniques are time consuming and require large amount of solvents, which are expensive, generate considerable waste, contaminate the sample and can enrich it for analytes. There have been many sample preparation techniques proposed to meet the requirements connected with the multiplicity of food. Optimal sample preparation can reduce analysis time, sources of error, enhance sensitivity and enable unequivocal identification and quantification. Sample extraction and purification techniques are discussed and their most recent applications in food analysis are provided. This review pointed out that sample preparation is the critical step. 相似文献
We have developed a metal‐free process for the aerobic photooxygenation of sulfides to sulfoxides mediated by riboflavin tetraacetate or riboflavin (vitamin B2) photocatalysts and visible light (450 nm) in an acetonitrile‐water (85:15 v/v) mixture. The optimised solvent system leads to both singlet‐oxygen and electron‐transfer pathways in photooxygenation, thus allowing oxidation of electron‐poor and electron‐rich thioanisoles, dialkyl sulfides and sterically hindered sulfides. Besides having a broad substrate scope, the method has very short reaction times and requires low catalyst loading (down to 0.1 mol%). These properties are due to the high photocatalyst stability and the extremely high quantum yields (1.3 for thioanisole oxygenation). Moreover, the method is chemoselective, producing only sulfoxides without overoxidation to sulfones. Taking into account the broad substrate scope, high selectivity and high efficiency, this method distinguishes itself from those previously reported. Other advantages include easy work‐up of the reaction mixture, the availability and biodegradability of the photocatalysts and mild reaction conditions. We demonstrated, on a preparative scale, its practical application in the synthesis of the psychostimulant modafinil, in the selective oxidation of methionine derivatives, and in the detoxification of mustard gas.
The phase transition observed by various methods in poly(vinyl methyl ether)/water systems at around 18 °C has been assigned by some investigators to the pre-melting of water and by others to a glass transition of the polymer. In this study, broadband dielectric spectroscopy and temperature modulated differential scanning calorimetry were used to identify this transition in radiationally crosslinked poly(vinyl methyl ether) hydrogels, as well as to analyse sub-zero relaxation processes in such a three-phase (polymer/ice/liquid water) system. The process at 18 °C was related to the pre-melting of water induced by the segmental motions of the polymer; however, it was seen to be one transition due to the cooperative motions of both compounds. The atypical (two regimes) temperature dependence of the segmental motion process was observed and was related to confinement of the polymer chains between ice clusters below approximately ?24 °C; furthermore, the main dielectric process of hexagonal ice was identified and a Maxwell-Wagner effect was observed. 相似文献