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  • Author or Editor: L. Wang x
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Abstract  

Thermal analysis of sulfurization of polyacrylonitrile (PAN) with elemental sulfur was investigated by thermogravimetry and differential thermal analysis of the mixture of polyacrylonitrile and elemental sulfur up to 600°C. Due to the volatilization of sulfur, the different heating rate (10 and 20 K min−1) and different mixture proportion of polyacrylonitrile and elemental sulfur were adopted to run the analysis. The different heating rates make the DSC curves of sulfur different, but make the DSC curves of PAN similar. In the DSC curve of sulfur for the heating rate of 20 K min−1 around 400°C, a small exothermic peak occurs at 400°C in the wide endothermic peak around 380∼420°C, indicative of that there is an exothermic reaction around 400°C. In the DSC curves of the mixture, the peaks around 320°C are exothermic as the content of sulfur is below 3.5:1 and endothermic as the content of sulfur is over 4:1, indicating that one of the reactions between PAN and sulfur takes place around 320°C. In the TG curves of the mixture, the mass losses begin at 220°C, and sharply drop down from 280°C. The curves for the low sulfur content obviously show two steps of mass loss, and curves for the high sulfur content show only one step of mass loss, indicative of more sulfur is benefit for the complete sulfurization of PAN. This study demonstrates that the TG/DSC analysis can give the parameter for the sulfurization, even if the starting mixture contains the volatile sulfur.

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Abstract  

The heat capacities of trans-(R)-3-(2,2-dichloroethenyl)-2,2-dimethylcyclopropanecarboxylic acid in the temperature range from 78 to 389 K were measured with a precise automatic adiabatic calorimeter. The sample was prepared with the purity of 0.9874 mole fraction. A solid-liquid fusion phase transition was observed in the experimental temperature range. The melting point, T m, enthalpy and entropy of fusion, Δfus H m, Δfus S m, were determined to be 344.75±0.02 K, 13.75±0.07 kJ mol−1, 39.88±0.21 J K−1 mol−1, respectively. The thermodynamic functions of the sample, H (T)-H (298.15), S (T)-S (298.15) and G (T)-G (298.15), were reported with a temperature interval of 5 K. The thermal decomposition of the sample was studied by TG analysis, the thermal decomposition starts at ca. 421 K and terminates at ca. 535 K, the maximum decomposition rate was obtained at 525 K. The order of reaction, pre-exponential factor and activation energy, are n=0.14, A=1.15·108 min−1, E=66.27 kJ mol−1, respectively.

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Summary

Chestnut exhibits anti-inflammatory, styptic, anti-diarrhea, and analgestic effects as a traditional Chinese medicine. There is increasing evidence that shows that the consumption of chestnuts has become more important in human nutrition due to the health benefits provided by the antioxidants. The phenolic compounds are responsible for major bioactivities, such as anti-tumor and anti-oxidation. A high-performance liquid chromatography (HPLC) method with diode array detection (DAD) was established for the simultaneous determination of six phenolic compounds (gallic acid, GA; protocatechuic acid, PR; catechin, CA; epicatechin, EP; quercetin, QU; kaempferol, KA) in Chinese chestnut (Castanea mollissima blume) kernel. The sample followed by separation on Eclipse XDB-C18 column (150 × 4.6 mm, id., 5 μm) with gradient elution of methanol-1.0% acetate acid solution as a mobile phase, at a temperature of 30°C, under the ratio of 1.2 mL min−1, with 5 μL injection volume, and multi-wavelength synthesis was used with DAD. The correlation coefficients were larger than 0.999, the recoveries were 97.58% for GA, 100.41% for PA, 96.23% for CA, 101.38% for QU, 99.15% for EP, and 98.60% for KA, relative standard deviation (RSD) were 1.04% for GA, 1.21% for PA, 1.09% for CA, 1.19% for QU, 1.06% for EP, and 1.20% for KA. This method was applied for the determination of phenolics in chestnut kernel and was found to be fast, sensitive, and suitable.

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Molecularly imprinted polymers (MIPs) were synthesized by imprinting a new template—S(-)-1,1′-binaphthalene-2,2′-diamine (S-DABN) and applied as chiral stationary phases for chiral separation of DABN racemates by high-performance liquid chromatography (HPLC). The influence of some key factors on the chiral recognition ability of MIPs, such as the type of functional monomers and porogen and the molar ratio of template to monomer, was systematically investigated. The chromatographic conditions, such as mobile phase composition, sample loading, and flow rate, were also measured. The chiral separation for DABN racemates under the optimum chromatographic conditions by using MIP chiral stationary phase (CSP) of P3, prepared with the S-DABN/MAA ratio = 1/4 and used acetonitrile (2 mL) and chloroform (4 mL) as porogen, showed the highest separation factor (2.14). Frontal analysis was used to evaluate affinity to the target molecule of MIPs. The binding sites (B t) of MIPs and dissociation constant (K d) were estimated as 4.56 μmol g−1 and 1.40 mmol L−1, respectively. In comparison with the previous studies, this approach had the advantages, such as the higher separation factor, easy preparation, and cost-effectiveness, it not only has the value for research but also has a potential in industrial application.

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Traditional Chinese medicine (TCM) has been widely used in many countries for thousands of years and played an indispensable role in the prevention and treatment of diseases, especially the complicated and chronic ones. However, the application of TCM in diseases is still not fully recognized by people around the world, the main reason is that Chinese herb is a very complex mixture containing hundreds of different components. Thus, it is essential to make quality control and evaluation of TCM. A new quality evaluation method, quantitative analysis of multi-components by single marker (QAMS), was developed to the quality control of alkaloids in TCM, a case study on Radix aconiti lateralis, named Fuzi in Chinese. Six alkaloids, including aconitine, hypaconitine, mesaconitine, benzoylaconine, benzoylmesaconine, and benzoylhypaconine, were selected as main components to evaluate the quality of Radix aconiti lateralis. The feasibility and accuracy of QAMS were checked by the external standard method, and various high-performance liquid chromatographic instruments and chromatographic conditions were investigated to verify its applicability. Using aconitine as the internal reference substance and the content of aconitine was calculated according to relative correction factors by high-performance liquid chromatography. The present results showed that there was no significant difference observed between the QAMS method and the external standard method with the relative average deviations less than 3.0%, and QAMS is an effective way to control the quality of herbal medicines and seems to be a convenient and accurate approach to analyze multi-composition when reference substances are unavailable.

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Summary

A preparative high-speed countercurrent chromatograph (HSCCC) method for the isolation and purification of C6-C2 natural alcohol and benzyl ethanol from Forsythia suspensa was successfully established. Cornoside, forsythenside F, forsythiaside, and acteoside were rapidly obtained for the first time by HSCCC with a two-phase solvent system ethyl acetate-n-butanol-methanol-water (5:1:0.5:5, υ/υ) in one-step separation. The purities of them were all above 97% as determined by high-performance liquid chromatography, and the combination of ESI-MS and NMR analysis confirmed the chemical structures of the four compounds.

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The chemical compositions of essential oils extracted by n-hexane extract (HE), petroleum ether extract (PE), dichloromethane extract (DE), and hydrodistillation (HD) from Carthamus tinctorius L. (safflower) were analyzed by gas chromatography-mass spectrometry (GC-MS). A total of 86 compounds from four different extracts were identified, and the contents were 97.65%, 98.05%, 98.93%, and 99.68%, respectively. 6,10,14-Trimethyl-2-pentadecanone, hexadecanoic acid, methyl ester, hexadecanoic acid, 8,11-octadecadienoic acid, methyl ester, and 9,12,15-octadecatrien-1-ol were the major constituents of the extracts. The antidiabete activity was assayed in vitro by against protein tyrosine phosphatase 1B (PTP1B). The results showed that the HE exhibited the best in vitro inhibitory enzyme activity against PTP1B, which holds a good potential for treating diabetes and obesity.

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This paper develops an instrumental analytical approach for detection of fourteen polycyclic aromatic hydrocarbons (PAHs) in edible oil samples using gel permeation chromatography (GPC) and ultra-high performance liquid chromatography (UHPLC) coupled with diode array detector (DAD), and fluorescence detector (FLD). The GPC was used to remove triglycerides from edible oil samples. The extracted samples were then detected using UHPLC—DAD—FLD. In order to obtain good separation and high reproducibility, the UHPLC—DAD—FLD experimental condition was optimized. The PAHs including three groups of isomeric PAHs can be separated completely in 12 min using BEH Shield RP 18 column with a suitable gradient elution program. The mean recoveries were in the range of 73–110% with an acceptable reproducibility (RSD < 10%, n = 3). During real sample analysis, the method can decrease the chance of false positives with both DAD and FLD being used simultaneously. The results indicate that the approach is simple, easy, and acceptably reproducible, thereby showing great potential as a method for detection of fourteen PAHs contained in edible oil samples.

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Summary

A new HPLC method has been established for determination of 3-monoiodotyrosine (MIT), 3,5-diiodotyrosine (DIT), 3,5-diiodothyronine (T2), 3,3′,5-triiodothyronine (T3), 3,3′,5′-triiodothyronine (rT3), and thyroxine (T4) produced by hydrolysis of iodinated casein with barium hydroxide. The hydrolytic stability of each analyte was evaluated. Iodinated casein was hydrolyzed with saturated barium hydroxide solution for 16 h at 110°C and the barium ions were then removed as barium sulfate. Reversed-phase HPLC was performed on a 2.1 mm × 150 mm, 5 μm particle, C18 column with a mixture of acetonitrile and 0.1% (v/v) formic acid as mobile phase at a flow rate of 0.2 mL min–1. Acetonitrile was maintained at 5% (v/v) for 5 min and then increased linearly to 50% (v/v) within 35 min. All analytes were quantified by measuring the absorbance at 280 nm. Validation data indicated the method was linear, with regression coefficients (R 2) > 0.998, in the concentration ranges investigated. Sensitivity was adequate—limits of detection (LOD) were 0.04–0.38 μg mL–1 and limits of quantification (LOQ) were 0.05–0.38 μg mL–1. Accuracy and precision were acceptable — for all the analytes recovery was 82.0–93.0% and repeatability, as relative standard deviation, was 1.0–3.0%. Hydrolytic stability tests indicated MIT and DIT are much more stable than the other analytes. rT3 was not released directly from iodinated casein but was formed by deiodination of T4 during hydrolysis. The method could be used to identify iodinated casein, to evaluate its activity and quality, and for supervision and regulation of feed additives.

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Soil seed banks can act as an important source in forest regeneration, and the information on the seed bank composition is vital for determining the resilience of plant communities under severe environments such as urban settings. In this study, we examined the seed bank density and functional composition, and their relationships with aboveground vegetation in three remnant evergreen broad-leaved forests, i.e., PuGang (PG), LuoGang (LG), and DaLingShan (DLS) under urbanization in Guangzhou, South China. In both years of our study (2010–2011), seed density and species richness for overall soil seed banks and each classified life forms (tree, shrub, herb and grass) significantly differed among the forests and were much higher in the PG forest. The prevailing life forms in the seed banks were herbs and grasses, and the proportion of tree species Importance Value index (IV) of the seed banks was low. We did not detect significant difference in the percentage of exotic species seeds in the seed banks among the forests. The proportion of species with animal dispersal mode was much higher in the DLS forest than in the PG and LG forests. The similarity in species composition between standing vegetation and seed banks was low with the lower value in the DLS forest than in PG and LG forest. Our findings suggest that the regeneration potential of the soil seed banks is limited for the remnant forests in urban areas. Therefore, greater proactive and enhanced conservation efforts are thus needed.

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