Hydrodynamic Radius Characterization of a Vinyl-Type Polynorbornene by Size-Exclusion Chromatography with a Static and Dynamic Laser Light Scattering Detector

Both absolute molecular weight and molecular sizes (radius of gyration and hydrodynamic radius) of a vinyl-type polynorbornene eluting from size-exclusion chromatography columns were determined by combined with a static and dynamic laser light scattering detector. The hydrodynamic radius of polymer fraction eluting from size-exclusion chromatography columns was obtained from dynamic laser light scattering measurements at only a single angle of 90° by introducing a correction factor. According to the scaling relationship between molecular sizes and molecular weight and the ratio between radius of gyration and hydrodynamic radius, the vinyl-type polynorbornene took a random coil conformation in 1,2,4-trichlorobenzene at 150 °C.     

Determination of vanadium, molybdenum and tungsten in complex matrix samples by chelation ion chromatography and on-line detection with inductively coupled plasma mass spectrometry

In this work, two kinds of chelating resin, bis(2-aminoethylthio)methylated resin (BAETM) and γ-aminobutyrohydroxamate resin (γ-ABHX) were synthesized. Of these, the former has a hydrophobic skeleton, and the latter a hydrophilic skeleton. The functionalities of each were 0.91 and 2.21 mmol g⁻¹, respectively. The chelating behavior of these resins towards vanadium, molybdenum and tungsten as a function of pH was studied. To perform trace metals analysis in complex matrices, a hyphenated method-chelation ion chromatography (CIC) coupled on-line detection with inductively coupled plasma mass spectrometry (ICP-MS) was developed. With a BAETM resin column (5×0.4 cm i.d.) as the separator, a sample volume of 20 μl, nitric acid (pH 1.5) as the eluent and a flow rate of 1 ml min⁻¹, the detection limits for the determination of vanadium, molybdenum and tungsten were lower than 0.05 ng ml⁻¹and the linear ranges were up to 100 ng ml⁻¹ for each element. By increasing the injected sample volume to 250 μl, the resin concentrator improved the detection limit to 0.01 ng ml⁻¹. For the determination of these elements (5 ng ml⁻¹ for each) spiked in artificial sea water samples, γ-ABHX resin column (3×0.6 cm i.d.) demonstrated well resolved peak separation between the analytes and the matrix elements—calcium and magnesium, by using sodium nitrate (10 ml, 10⁻⁴ M) as the eliminator.     

Derivatization of carboxylic acids with 9-bromomethylacridine using micellar phase-transfer catalysis

Summary Micellar phase-transfer catalysis (MPTC) offers the opportunity to derivatize carboxylic acids directly in an aqueous matrix without prior extraction of the acids into a suitable aprotic solvent. The currently developed MPTC system consists of a non-ionic surfactant, Arkopal N-130, an ion-pair agent, tetrakis-(decyl)-ammonium bromide, and a novel fluorescence reagent, 9-bromomethylacridine. The MPTC system can be applied to the derivatization of many types of carboxylic acids. The reaction rate is affected by the lipophilicity of the acid and by the presence of other functional groups. For lipophilic carboxylic acids the reaction is complete within 5 min at 60°C and pH 7.0.     

生物质裂解产物的制备及HPLC检测其成分的虚拟仿真实验开发

In order to improve university laboratory teaching and practical education under the background of information technology, as well as overcome the difficulty for practical training, develop a virtual simulation experiment platform for rapid pyrolysis of natal materials and high-performance liquid chromatographic (HPLC) detection of its components. The experiment integrates the actual operation process of the plant to produce cleaved products by rapid pyrolysis of biomass with HPLC detection. The virtual experiment is divided into biomass sample pretreatment, rapid biomass pyrolysis, bio-oil extraction, and HPLC determination of complex components, making the biomass cleavage workshop "real" through simulation. This virtual simulation experiment fully integrates the utilization of biomass resources and basic chemistry courses (such as organic chemistry, instrumental analysis, chemical engineering principles, etc.), which are widely involved in agricultural and forestry majors with advantageous characteristics value.     

磁性纳米标记检测技术在生物医学即时检测领域的研究进展

基于磁性纳米材料的磁标记检测技术具有灵敏度高、线性范围广、信号检测便捷等优点。由于生物样品自身磁背景信号极低,相比于光学标记检测技术,磁标记检测技术在蛋白质、核酸、细胞、病原体及生物组织检测中均表现出更高的灵敏度,在生物医学即时检测领域展现了良好的应用前景。该文围绕磁性纳米粒在即时检测领域的最新研究进展,重点介绍了其在蛋白质、核酸以及几类病原体检测方面的应用,并对基于磁性纳米粒的即时检测技术发展方向及应用前景进行了展望。     

Chromatographic Analysis of Trans Resveratrol in Italian Wines: Comparisons between FL, UV and MS Detection

Resveratrol (3,5,4′-trihydroxystilbene) is a phytoalexin that belongs to the group of stilbenes, known to occur in grapes and consequently in grape products. Its presence in wine is an important qualitative parameter because of the several beneficial effects on human health. The aim of this work is the development of a high-performance liquid chromatographic (HPLC) method for the determination of trans resveratrol in wines, and comparisons between the results obtained by different detection techniques: UV-vis spectroscopy, fluorescence spectroscopy and mass spectrometry. Resveratrol is analysed on a C-18 column using gradient elution. The method permits direct injection of sample, revealing to be time-saving, overcoming the need of sample pre-treatment steps. Detection limits were 154.8 ng mL⁻¹ by HPLC-UV, 118.0 ng mL⁻¹ by HPLC-FL and 48.0 ng mL⁻¹ by HPLC-MS. Trans resveratrol has been then quantified in a group of 52 wines derived from different Italian regions, cultivars and winemaking technologies by HPLC-UV.     

Detection and assessment of citrus tristeza virus antigens by computer-aided scanning densitometry

Citrus tristeza virus (CTV) extracted from Etrog citron (C.medica L.) was immunoprecipitated. The immunoprecipitate was fractionated by SDS-PAGE and western blotted onto nitrocellulose. The CTV antigens were determined by immunoblot analysis using rabbit anti-CTV IgG, and the protein-band pattern exhibited on the nitrocellulose was assessed by soft-laser scanning densitometry. The densitometric tracing revealed the presence of bands that were not visible to the naked eye. Using the superimposition mode of the instrument, it was also revealed that the protein-band patterns of different CTV samples were not identical. Computer-aided soft-laser scanning densitometry proved to be a powerful approach in the detection and assessment of protein bands revealed on nitrocellulose immunoblots, which we were previously unable to do employing conventional methods.     

毛细管电泳安培法检测中的在柱场放大效应

本文首次报道用安培电化学检测器探讨毛细管电泳分离的场放大进样效应，分析了系统峰的形成以及场放大进样对电泳分离检测的影响。采用２５μｍ内径毛细管电泳分离，对去甲肾上腺素（ＮＥ）和儿茶酚（ＣＡＴ）分别可达０．４ｎｍｏｌ／Ｌ和１．５ｎｍｏｌ／Ｌ的浓度检测限，有效提高了毛细管电泳安培法检测的灵敏度。     

Cloud point extraction of napropamide and thiabendazole from water and soil

The micellar extraction and enrichment of napropamide and thiabendazole using Genapol X 80 is described. Combined with their quantification by fluorescence, detection limits below 0.2 g/l with recovery rates of up to 95% were achieved. The recovery could be improved by lowering the extraction temperature and purificaton of the surfactants. This extraction method has been applied to the isolation and preconcentration of napropamide from standard soils. Experimental parameters affecting the recovery rates were examined.     

Mass distribution in a dynamic sample zone inside a flow injection manifold: modelling integrated conductimetric profiles

A mathematical model for fitting the experimental ICM (integrated conductimetric method) curves developed by the authors in a previous work, is presented for the first time in this study. The proposed model fits the experimental curves with great precision and allows to predict physical dispersion for single-line flow injection system. The correlation of the model’s parameters with typical reactionless FIA peak parameters is also assessed. The IDQ coefficient—a novel dispersion estimator previously reported by the authors—can also be predicted when operational FIA variables are changed. Experimental and modelled profiles are compared as a function of the system’s variables, showing an excellent agreement.