A newly-developed method of complete separation and sensitive determination of o-, m-, and p-aminobenzoic acid isomers was achieved by combining open-tubular columns for capillary electrochromatography (OT-CEC) and online sample stacking. In this study, spherical gold nanoparticles were modified by a covalent attachment of mono-6-thio-β-cyclodextrin, and OT-CEC was formed by immobilizing cyclodextrin-modified gold nanoparticles (CD-AuNP) on prederivatized 3-mercaptopropyl-trimethoxysilane fused-silica capillaries. Based on the theory of moving chemical reaction boundary, effects of several important factors such as the pH and concentration of running buffer and the conditions of stacking analytes were optimized. The optimized separations were carried out in 58 mmol/L HAc buffer at pH 3.0 using a capillary coated with CD-AuNP, while the optimized concentration was carried out in 50 mmol/L disodium hydrogen phosphate (pH 9.5). The linear ranges for m-, p-, and o-aminobenzoic acid were from 5.0 × 10−4–0.1, 5.0 × 10−4–0.1 and 1.0 × 10−4–0.1 mmol/L, respectively. And the detection limits (S/N = 3) were as low as 8.22 × 10−5, 8.21 × 10−5, and 3.76 × 10−5 mmol/L for m-, p-, and o-aminobenzoic acid, respectively. The run-to-run, day-to-day, and column-to-column reproducibilities of migration time were satisfactory with relative standard deviation values of less than 4.5 % in all cases. This method was successfully used in determining procaine hydrochloride injection sample with recoveries in the range of 96.1–106.6 % and relative standard deviations less than 5.0 %.
A newly-developed method of complete separation and sensitive determination of o-, m-, and p-aminobenzoic acid isomers was achieved by combining open-tubular columns for capillary electrochromatography (OT-CEC) and online sample stacking. In this study, spherical gold nanoparticles were modified by a covalent attachment of mono-6-thio-β-cyclodextrin, and OT-CEC was formed by immobilizing cyclodextrin-modified gold nanoparticles (CD-AuNP) on prederivatized 3-mercaptopropyl-trimethoxysilane fused-silica capillaries. Based on the theory of moving chemical reaction boundary, effects of several important factors such as the pH and concentration of running buffer and the conditions of stacking analytes were optimized. The optimized separations were carried out in 58 mmol/L HAc buffer at pH 3.0 using a capillary coated with CD-AuNP, while the optimized concentration was carried out in 50 mmol/L disodium hydrogen phosphate (pH 9.5). The linear ranges for m-, p-, and o-aminobenzoic acid were from 5.0 × 10?4–0.1, 5.0 × 10?4–0.1 and 1.0 × 10?4–0.1 mmol/L, respectively. And the detection limits (S/N = 3) were as low as 8.22 × 10?5, 8.21 × 10?5, and 3.76 × 10?5 mmol/L for m-, p-, and o-aminobenzoic acid, respectively. The run-to-run, day-to-day, and column-to-column reproducibilities of migration time were satisfactory with relative standard deviation values of less than 4.5 % in all cases. This method was successfully used in determining procaine hydrochloride injection sample with recoveries in the range of 96.1–106.6 % and relative standard deviations less than 5.0 %. 相似文献
A new molecularly imprinted polymer (MIP) has been prepared on silica beads using the radical “grafting from” polymerization
method for selective extraction of minor contaminant mycotoxin of patulin (PTL). After the introduction of amino groups onto
the silica surface with 3-aminopropyltriethoxysilane, azo initiator onto the silica surface was achieved by the reaction of
surface amino groups with 4,4′-azobis(4-cyanopentanoic acid). The scale-up synthesis of MIP was then carried out in the presence
of 6-hydroxynicotinic acid as template substitute, functional, and cross-linking monomers. The prepared sorbent was characterized
using FT-IR spectroscopy, scanning electron microscopy, elemental analysis, and the adsorption–desorption selectivity, and
the capacity characteristic of the polymer was investigated by a conventional batch adsorption test and Scatchard plot analysis.
The results indicated that coated polymers had specific adsorption to PTL as compared with its co-occurring 5-hydroxymethyl-2-furaldehyde
(hydroxymethylfurfural (HMF)), at the same bulk concentration for solution of PTL and HMF, the maximum absorbance in the solid-phase
extraction (SPE) method to PTL were 93.97% or 0.654 μg/mg while to HMF they were 76.89% or 0.496 μg/mg. Scatchard analysis
revealed that two classes of binding sites were formed in PTL-MIP with dissociation constants of 3.2 × 10−2 and 5.0 × 10−3 mg/mL and the affinity binding sites of 8.029 and 1.364 mg/g, respectively. The recoveries of PTL were more than 90% for
the developed MISPE and around 75% for the traditional liquid–liquid extraction in spiked apple juice samples. It was concluded
that the method is suitable for the scale-up synthesis of PTL-MIP grafted on silica, and the polymer can be effectively applied
as SPE coupled with high-performance liquid chromatography (HPLC) for the determination of PTL in apple juice or other related
products. 相似文献
Dynamic states of cancer cells moving under shear flow in an antibody-functionalized microchannel are investigated experimentally and theoretically. The cell motion is analyzed with the aid of a simplified physical model featuring a receptor-coated rigid sphere moving above a solid surface with immobilized ligands. The motion of the sphere is described by the Langevin equation accounting for the hydrodynamic loadings, gravitational force, receptor-ligand bindings, and thermal fluctuations; the receptor-ligand bonds are modeled as linear springs. Depending on the applied shear flow rate, three dynamic states of cell motion have been identified: (i) free motion, (ii) rolling adhesion, and (iii) firm adhesion. Of particular interest is the fraction of captured circulating tumor cells, defined as the capture ratio, via specific receptor-ligand bonds. The cell capture ratio decreases with increasing shear flow rate with a characteristic rate. Based on both experimental and theoretical results, the characteristic flow rate increases monotonically with increasing either cell-receptor or surface-ligand density within certain ranges. Utilizing it as a scaling parameter, flow-rate dependent capture ratios for various cell-surface combinations collapse onto a single curve described by an exponential formula. 相似文献
This paper computes the Thom map on γ2 and proves that it is represented by 2b2,0h1,2 in the ASS. The authors also compute the higher May differential of b2,0, from which it is proved that (~γ)s(b0hn - h1bn-1) for 2 ≤ s < p - 1 are permanent cycles in the ASS. 相似文献
Let be the canonical framework of white noise analysis over the Gel'fand triple and be the space of continuous linear operators from to . Let be a self-adjoint operator in with spectral representation . In this paper, it is proved that under appropriate conditions upon , there exists a unique linear mapping such that for each . The mapping is then naturally used to define as , where is the Dirac -function. Finally, properties of the mapping are investigated and several results are obtained.
The level set method is commonly used to address image noise removal. Existing studies concentrate mainly on determining the speed function of the evolution equation. Based on the idea of a Canny operator, this letter introduces a new method of controlling the level set evolution, in which the edge strength is taken into account in choosing curvature flows for the speed function and the normal to edge direction is used to orient the diffusion of the moving interface. The addition of an energy term to penalize the irregularity allows for better preservation of local edge information. In contrast with previous Canny-based level set methods that usually adopt a two-stage framework, the proposed algorithm can execute all the above operations in one process during noise removal. 相似文献