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Long Z.,Xinjiang Uygur Autonomous Region Product Quality Supervision and Inspection Institute | Ma N.,CAS Lanzhou Institute of Chemical Physics | Wu B.,CAS Lanzhou Institute of Chemical Physics
Bulletin of the Korean Chemical Society | Year: 2011

A self-assembled Al-bridged diiminopyridine-based ligand (3) was synthesized and characterized by FT-IR, ESI-MS and NMR spectroscopy. Electron spectral titrations were performed to confirm the formation of a novel trinuclear bis(imino)pyridyl iron(II) complex (4) upon addition of FeCl 2 into Al-bridged ligand 3 in methanol solution. Simultaneously, a typical bis(imino)pyridine-iron(II) complex (2) was synthesized and fully characterized. The X-ray crystal study of the iron(II) complex 2 disclosed a five-coordinate, distorted squarepyramidal structure with the tridentate N^N^N ligand and chlorides. The optimal molecular structure of 4 was obtained by means of molecular mechanics, which showed that each iron atom in the complex 4 is surrounded by two chlorides, a tridentate N^N^N ligand and one oxygen atom, supporting considerations about the possibility of six-coordinate geometry from MMAO or the ethylene access. A comparison of 4 with the reference 2 revealed a remarkable decrease of the catalytic activity and MMAO consumption (activity up to 0.41 × 103 kg molFe -1 h-1 bar-1, Al/Fe = 650 for 4 and 7.02 × 103 kg molFe -1 h-1 bar-1, Al/Fe = 1600 for 2).


Wu D.-T.,University of MacauMacao | Lam S.-C.,University of MacauMacao | Cheong K.-L.,University of MacauMacao | Wei F.,National Institutes for Food and Drug Control | And 7 more authors.
Journal of Pharmaceutical and Biomedical Analysis | Year: 2016

Molecular weights and contents of water-soluble polysaccharides and their fractions in fifty batches of fruits of Lycium barbarum (wolfberry) collected from different regions of China, including Qinghai, Ningxia, Inner Mongolia, Xinjiang, and Gansu, were simultaneously determined using high performance size exclusion chromatography (HPSEC) coupled with multi angle laser light scattering (MALLS) and refractive index detector (RID) with the refractive index increment (dn/dc). Results showed that HPSEC chromatograms and molecular weight distributions of polysaccharides in L. barbarum collected from different regions of China were similar. Furthermore, the average contents of each polysaccharide fraction (peaks 1, 2, and 3) in crude polysaccharides of L. barbarum collected from Ningxia were similar with those of Inner Mongolia, Xinjiang, and Gansu, respectively. However, significant difference was found between polysaccharides in L. barbarum collected from Ningxia and Qinghai. Moreover, the average amounts of total polysaccharide fractions (peaks 1, 2, and 3) in the raw material of L. barbarum collected from Ningxia were significantly higher than that of Qinghai. These results may contribute to the rational usage of L. barbarum produced in China, and are beneficial for the improvement of their quality control. Results suggested that HPSEC-MALLS-RID with the dn/dc method could be used as a routine method for the quality evaluation of polysaccharides from natural resources and their products. © 2016 Elsevier B.V.


Jian L.-J.,Xinjiang Uygur Autonomous Region Product Quality Supervision and Inspection Institute | Chang J.-M.,Xinjiang Medical University | Ablise M.,Xinjiang Medical University | Li G.-R.,Xinjiang Medical University | He J.-W.,Xinjiang Medical University
Journal of Asian Natural Products Research | Year: 2014

The polysaccharide extract (PE) of Uyghur medicinal preparation Alhagi-honey was prepared by water extraction and alcohol precipitation method. The purified polysaccharide AP1-1 was obtained from PE by macroporous adsorption resin chromatography, DEAE cellulose chromatography, and Sephadex gel chromatography; the homogeneity and the molecular weight of AP1-1 were determined by gel filtration; and the acid hydrolysis, periodate oxidation, Smith degradation, and NMR analysis were used to analyze the chemical structure of AP1-1. The result showed that AP1-1 was a homogeneous polysaccharide, whose relative molecular weight was 9.97 × 104. Through high-performance capillary electrophoresis analysis, we found that its molecular structure was composed of mannose, glucose, galactose, and galacturonic acid with a molar ratio of about 1.1:1.9:3.9:2.1. The main chain of AP1-1 was mainly made up of → 4)β-d-GalpA-(1 → 4)β-d-GalpA-(1 → 4)-β-d-Galp-(1 → 4)-β-d-Galp-(1 → 6)-d-Glcp-(1 → 4)-d-Glcp(1 →, while the side chain is composed of → 6)-d-Glcp and 2-CH3-d-Man. © 2014 © 2014 Taylor & Francis.


Wu D.-T.,University of Macau | Cheong K.-L.,University of Macau | Deng Y.,University of Macau | Lin P.-C.,Qinghai University for Nationalities | And 7 more authors.
Carbohydrate Polymers | Year: 2015

Water-soluble polysaccharides from 51 batches of fruits of L. barbarum (wolfberry) in China were investigated and compared using saccharide mapping, partial acid hydrolysis, single and composite enzymatic digestion, followed by polysaccharide analysis by using carbohydrate gel electrophoresis (PACE) analysis and high performance thin layer chromatography (HPTLC) analysis, respectively. Results showed that multiple PACE and HPTLC fingerprints of partial acid and enzymatic hydrolysates of polysaccharides from L. barbarum in China were similar, respectively. In addition, results indicated that β-1,3-glucosidic, α-1,4-galactosiduronic and α-1,5-arabinosidic linkages existed in polysaccharides from L. barbarum collected in China, and the similarity of polysaccharides in L. barbarum collected from different regions of China was pretty high, which are helpful for the improvement of the performance of polysaccharides from L. barbarum in functional/health foods area. Furthermore, polysaccharides from Panax notoginseng, Angelica sinensis, and Astragalus membranaceus var. mongholicus were successfully distinguished from those of L. barbarum based on their PACE fingerprints. These results were beneficial to improve the quality control of polysaccharides from L. barabrum and their products, which suggested that saccharide mapping based on PACE and HPTLC analysis could be a routine approach for quality control of polysaccharides. © 2015 Elsevier Ltd. All rights reserved.


Long Z.,Xinjiang Uygur Autonomous Region Product Quality Supervision and Inspection Institute | Xu W.,Xinjiang University | Lu Y.,Xinjiang Uygur Autonomous Region Product Quality Supervision and Inspection Institute | Qiu H.,CAS Lanzhou Institute of Chemical Physics
Journal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences | Year: 2016

A new and facile rhodamine B (RhB)-imprinted polymer nanoshell coating for SiO2 nanoparticles was readily prepared by a combination of silica gel modification and molecular surface imprinting. The RhB-imprinted polymers (RhB-MIPs) were characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, and UV-vis spectroscopy; the binding properties and selectivity of these MIPs were investigated in detail. The uniformly imprinted nanoparticles displayed a rather thin shell thickness (23nm) with highly effective recognition sites, showing homogenous distribution and monolayer adsorption. The maximum MIP adsorption capacity (Q m) was as high as 45.2mgg-1, with an adsorption equilibrium time of about 15min at ambient temperature. Dynamic rebinding experiments showed that chemical adsorption is crucial for RhB binding to RhB-MIPs. The adsorption isotherm for RhB-MIPs binding could also be described by the Langmuir equation at different temperatures and pH values. Increasing temperature led to an enhanced Q m, a decreased dissociation constant (K' d), and a more negative free energy (δG), indicating that adsorption is favored at higher temperatures. Moreover, the adsorption capacity of RhB was remarkably affected by pH. At pH>7, the adsorption of RhB was driven by hydrogen bonding interactions, while at pH<7 electrostatic forces were dominant. Additionally, the MIPs also showed specific recognition of RhB from the standard mixture solution containing five structurally analogs. This method was also successfully employed to determine RhB content in red wine and beverages using three levels of spiking, with recoveries in the range of 91.6-93.1% and relative standard deviations lower than 4.1%. © 2016 Elsevier B.V.

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