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排序方式: 共有195条查询结果,搜索用时 15 毫秒
191.
Emiliano De Dominicis Italo Commissati Elisa Gritti Dante Catellani 《Food additives & contaminants. Part A, Chemistry, analysis, control, exposure & risk assessment》2015,32(10):1617-1627
In addition to ‘traditional’ multi-residue and multi-contaminant multiple reaction monitoring (MRM) mass spectrometric techniques devoted to quantifying a list of targeted compounds, the global food industry requires non-targeted methods capable of detecting other possible potentially hazardous compounds. Ultra-high-performance liquid chromatography combined with a single-stage Orbitrap high-resolution mass spectrometer (UHPLC-HRMS Exactive?-Orbitrap Technology) was successfully exploited for the complete selective and quantitative determination of 33 target compounds within three major cross categories (pesticides, antibiotics and mycotoxins) in bakery matrices (specifically milk, wheat flour and mini-cakes). Resolution was set at 50 000 full width at half maximum (FWHM) to achieve the right compromise between an adequate scan speed and selectivity, allowing for the limitations related to the necessary generic sample preparation approach. An exact mass with tolerance of 5 ppm and minimum peak threshold of 10 000 units were fixed as the main identification conditions, including retention time and isotopic pattern as additional criteria devoted to greatly reducing the risk of false-positive findings. The full validation for all the target analytes was performed: linearity, intermediate repeatability and recovery (28 analytes within 70–120%) were positively assessed; furthermore, limits of quantification between 5 and 100 µg kg?1 (with most of the analytes having a limit of detection below 6 µg kg?1) indicate good performance, which is compatible with almost all the regulatory needs. Naturally contaminated and fortified mini-cakes, prepared through combined use of industrial and pilot plant production lines, were analysed at two different concentration levels, obtaining good overall quantitative results and providing preliminary indications of the potential of full-scan HRMS cluster analysis. The effectiveness of this analytical approach was also tested in terms of the formulation of hypotheses for the identification of other analytes not initially targeted which can have toxicological implications (e.g. 3-acetyl-deoxynivalenol and deoxynivalenol-3-glucoside), opening a window on retrospective investigation perspectives in food safety laboratories. 相似文献
192.
Dimethyl ether (DME) homologation forms isobutane and triptane (2,2,3-trimethylbutane) with supra-equilibrium selectivities within C4 and C7 hydrocarbons on both mesoporous solid acids (SiO2–Al2O3, H3PW12O40/SiO2) and the acid forms of various zeolites (BEA, FAU, MFI) via methylation and hydride transfer steps that favor isobutane and triptane formation because of the relative stabilities of ion-pairs at transition states for chains along the preferred growth path. The stabilities of ion-pair transition states increase as acid sites become stronger and energies for charge separation decrease and as van der Waals interactions within pores become stronger, which respectively lead to higher rates on H3PW12O40/SiO2 and aluminosilicate zeolites than on amorphous SiO2–Al2O3. Solid acids with different strengths and abilities to solvate ion-pairs by confinement differ in selectivity because strength and solvation influence transition states for the hydride transfer, methylation, and isomerization steps to different extents. Stronger acid sites on H3PW12O40/SiO2 favor isomerization and hydride transfer over methylation; they lead to higher selectivities to n-butane and non-triptane C7 isomers than the weaker acid sites on BEA, FAU, and mesoporous SiO2–Al2O3. This preference for hydride transfer and isomerization on stronger acids reflects transition states with more diffuse cationic charge, which interact less effectively with conjugate anions than more localized cations at methylation transition states. The latter recover a larger fraction of the energy required to form the ion-pair, and their stabilities are less sensitive to acid strength than for diffuse cations. Large-pore zeolites (BEA, FAU) form triptane with higher selectivity than SiO2–Al2O3 because confinement within large pores preferentially solvates the larger transition states for hydride transfer and methylation, which preserve the four-carbon backbone in triptane, over smaller transition states for alkoxide isomerization steps, which disrupt this backbone and cause growth beyond C7 chains and subsequent facile β-scission to form isobutane. MFI forms isobutane and triptane with much lower selectivity than mesoporous acids or large-pore zeolites, because smaller pores restrict the formation of bimolecular methylation and hydride transfer transition states required for chain growth and termination steps to a greater extent than those for monomolecular alkoxide isomerization. These data and their mechanistic interpretations show that the selective formation of isobutane and triptane from C1 precursors like DME is favored on all acids as a result of the relative stability of methylation, hydride transfer, and isomerization transition states, but to a lesser extent when small confining voids and stronger acid sites preferentially stabilize monomolecular isomerization transition states. The observed effects of acid strength and confinement on rates and selectivities reflect the more effective stabilization of all ion-pairs on stronger acids and within solvating environments, but a preference for transition states with more diffuse charge on stronger acids and for ion-pairs with the appropriate solvation within voids of molecular dimensions. 相似文献
193.
Luciano E. Chiang Dante A. Elías 《International Journal of Rock Mechanics and Mining Sciences》2008,45(5):701-711
A three-dimensional (3D) finite element approach for modeling impact as it occurs in impact tools used in rock drilling is presented. The model permits one to simulate the energy transmission to the rock, the bit–rock interaction, and the process of rock fragmentation, all of which are important in the study and evaluation of such tools. The finite elements method (FEM) analysis allows one to simulate the impact in 3D stress–strain problems, to consider linear material properties, and to include post failure fracture propagation. Anisotropic elements have been used to model the rock post failure behavior. Infinite domain elements have been used to characterize boundary conditions far away from bit–rock interaction. The accuracy of the model has been evaluated both theoretically by comparing the result to those obtained with a model based on impulse–momentum principle as well as experimentally. 相似文献
194.
Synthesis and corrosion inhibition of α-amino acids alkylamides for mild steel in acidic environment
O. Olivares-Xometl N.V. Likhanova M.A. Domínguez-Aguilar E. Arce H. Dorantes P. Arellanes-Lozada 《Materials Chemistry and Physics》2008,110(2-3):344-351
New compounds of alkylamides derived from α-amino acids were tested as corrosion inhibitors for carbon steel in an aqueous solution of hydrochloric acid. The chemical synthesis of these amides performed by aminolysis of α-amino acid methyl esters resulted in good yields. Electrochemical testing was carried out using polarization scans and weight loss measurements. Polarization scans indicated that compounds act as mixed corrosion inhibitors with an efficiency of 80–90% when dissolved in the testing solution at ≥50 ppm, whereas gravimetric results displayed a similar tendency. Microtox testing indicated a correlation with the molecular structure of inhibitors. Apparently, a long aliphatic chain (C > 12) promoted not only higher corrosion efficiency, but also a higher toxicity. The higher efficiency of dodecyl amine of tyrosine was apparently derived from its longer aliphatic chain, with some contribution from its phenyl ring, which reinforces the molecular interactions of π type bonding to the d orbital metal favouring film formation. 相似文献
195.
基于面内补偿的微机电系统离面运动测试 总被引:1,自引:1,他引:0
将频闪成像技术和相移显微干涉技术相结合,提出了一种基于面内补偿的微机电系统(MEMS)离面运动测试方法。首先通过相移显微干涉技术自动采集MEMS结构运动周期内不同准静态位置处的数帧相移干涉图像;然后通过图像处理得到每个准静态位置的亮场图像,进行面内位移测试;最后利用面内位移测试结果对离面位移测试进行补偿,即双相位展开算法,完成对于MEMS结构的离面运动测试。实验结果表明:面内运动的测试的精度可达0.01 pixel,静态离面高度测试的重复精度可达0.52 nm,可以完成伴随着面内位移的MEMS离面位移测试。 相似文献