JOURNAL OF SEPARATION SCIENCE
·
2016
·Vol. 39
·期 12
·2413-2421
·
IF 2.741
Chao Han,Jianguang Luo,Zhongrui Li,Yingqi Zhang,Huijun Zhao,Lingyi Kong
A biphasic chiral recognition system based on chiral ligand exchange with Cu(II)- N - n -dodecyl-L-proline and hydroxypropyl-β-cyclodextrin as an additive was developed to enantioseparate aromatic β-amino acids by high-speed counter-current chromatography. The biphasic chiral recognition system was established with an n -butanol/water (1:1, v/v) solvent system by adding N - n -dodecyl-L-proline and Cu(II) ions to the organic phase and hydroxypropyl-β-cyclodextrin to the aqueous phase. Several separation parameters, such as temperature, pH value, and chiral selector concentration, were systematically investigated by enantioselective liquid–liquid extraction. Under the optimal separation conditions, 54.5 mg of ( R , S )-β-phenylalanine and 74.3 mg of ( R , S )-β-3,4-dimethoxyphenylalanine were baseline enantioseparated. More importantly, the synergistic enantiorecognition mechanism, based on the Cu(II)- N - n -dodecyl-L-proline and hydroxypropyl-β-cyclodextrin, was discussed for the first time.
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TALANTA
·
2017
·
IF 4.162
Liang Li,Biaoping Cheng,Rendan Zhou,Zhigang Cao,Chun Zeng,Laisheng Li
A novel N -benzyl-phenethylamino-β-cyclodextrin-bonded ordered mesoporous SBA-15 chiral stationary phase (BZCDP) for high-performance liquid chromatography (HPLC) was prepared. The structure and morphology of the ligand and the stationary phase were characterized by mass spectrometry, elemental analysis , infrared spectroscopy, scanning electron microscopy, transmission electron microscopy and thermogravimetric analysis . The enantiomers of chiral compounds including nine common β-adrenergic blocker drugs (β-blockers), eight dansyl amino acids (DNS-AA) and six flavanones were successfully separated by polar organic solvent and reversed-phase chromatography, respectively. The results showed that BZCDP was a kind of multimode chiral separation materials with an excellent chromatographic performance for the above compounds. In polar organic solvent mode, BZCDP can effectively separate β-blockers, in which the enantioselectivity factors and resolutions of β-blockers were up to 1.30 and 1.97 within 20 min, respectively. Under the reversed-phase mode, BZCDP exhibited high enantioselectivities for DNS-AA, among them the resolution of dansyl-tyrosine was 3.29 with 20 min. BZCDP was also successfully used to separate the flavanone compounds with methanol or acetonitrile as mobile phase . The resolution of 4'-hydroxy flavanone enantiomers reached to 3.65 about 15 min. Compared with the native β-cyclodextrin and γ-cyclodextrin-bonded stationary phases in the literature, the separation speed of BZCDP containing mono - N -benzyl-phenethylamino-β-cyclodextrin ligand was faster and the separation selectivity was better, which indicated that the N -benzyl-phenethylamino group could also take part in the chiral recognition. After further study, we found that in polar organic solvent mode, the inclusion and hydrogen bonding were the main forces of chiral separations, and in reversed-phase mode, the inclusion and hydrophobic interaction are the main driving forces for chiral separations. Besides excellent chromatographic performance, the home-made cyclodextrin column with mesoporous SBA-15 as the matrix was much cheaper than commercial columns, and good permeability, which can reduce the cost of test and provide fast separation. BZCDP has a good prospect in chiral drug analysis.
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TALANTA
·
2016
·
IF 4.035
Jialiang Guo,Yuan Xiao,Yuanjing Lin,Qiaoxuan Zhang,Yiqun Chang,Jacques Crommen,Zhengjin Jiang
In order to investigate the effect of the linking spacer on the enantioseparation ability of β -cyclodextrin ( β -CD) functionalized polymeric monoliths, three β -CD-functionalized organic polymeric monoliths with different spacer lengths were prepared by using three amino- β -CDs, i.e. mono-6-amino-6-deoxy- β -CD, mono-6-ethylenediamine-6-deoxy- β -CD, mono-6-hexamethylenediamine-6-deoxy- β -CD, as starting materials. These amino- β -CDs reacted with glycidyl methacrylate to produce functional monomers which were then copolymerized with ethylene dimethacrylate. The enantioseparation ability of the three monoliths was evaluated using 14 chiral acidic compounds, including mandelic acid derivatives, nonsteroidal anti-inflammatory drugs, N -derivatized amino acids , and chiral herbicides under optimum chromatographic conditions. Notably, the poly(GMA-NH 2 - β -CD- co -EDMA) column provides higher enantioresolution and enantioselectivity than the poly(GMA-EDA- β -CD- co -EDMA) and poly(GMA-HDA- β -CD- co -EDMA) columns for most tested chiral analytes. Furthermore, the enantioseparation performance of triazole-linker containing monoliths was compared to that of ethylenediamine-linker containing monoliths. The results indicate that the enantioselectivity of β -CD monolithic columns is strongly related to the length and type of spacer tethering β -CD to the polymeric support .
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JOURNAL OF SOLID STATE ELECTROCHEMISTRY
·
2016
·Vol. 20
·期 5
·1377-1389
·
IF 2.327
Hui Yuchen,Ma Xiaoyan,Qu Fengjin,Chen Fang,Yu Jie,Gao Yan
A facile strategy is developed to fabricate an Au-CMCD/PCMCD electrode with high efficiency, universal, and selectivity electrocatalysis through electro-depositing carboxymethyl-β-cyclodextrins with gold nanoparticles (Au-CMCD) followed by employing electro-polymerization carboxymethyl-β-cyclodextrin (PCMCD). The chemical structure, microstructure, electrochemical activity, and electrocatalytic properties of Au-CMCD/PCMCD electrode are investigated. Due to the synergistic effect of the PCMCD and Au-CMCD layers, the as-prepared electrode exhibits an outstanding enhancement of universal electrocatalytic activity to eight kinds of crucial biomolecules and drugs, such as chloramphenicol, thymine, and glucose. Then, as a target analyte, glucose is used to investigate the sensing performances of Au-CMCD/PCMCD electrode. The amperometric detection of glucose shows a wide linear range expanding to 0.001∼110 mM with a low detection limit of 0.99 μM. More importantly, the absorption effect of PCMCD is stronger to glucose than other interfering species, which is favorable to avoid the influence of possible interfering substances. Furthermore, the glucose sensors reveal good stability and repeatability.
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JOURNAL OF SEPARATION SCIENCE
·
2017
·Vol. 40
·期 19
·3754-3762
·
IF 2.557
Yuanjing Lin,Jialiang Guo,Hang Lin,Jincai Wang,Govert W. Somsen,Jacques Crommen,Zhengjin Jiang
To evaluate the effect of the preparation strategy on the enantioseparation performance of β-cyclodextrin-functionalized monoliths, a series of β-cyclodextrin-functionalized organic polymeric monolithic columns were prepared through two-step, single-step, and one-pot approaches, using the same cyclodextrin, linker–spacer, and crosslinker. Physicochemical characterization of the columns was carried out by determining the morphology, β-cyclodextrin density, permeability, and chromatographic efficiency. For each type of monolithic column, the enantioresolution of 22 chiral compounds, including mandelic acid derivatives, nonsteroidal anti-inflammatory drugs, N-derivatized amino acids, and herbicides, was comparatively studied under optimum chromatographic conditions. The β-cyclodextrin-functionalized monolithic columns prepared through the one-pot approach exhibited higher enantioresolution for most chiral compounds, and they have the advantage of good controllability and simple preparation. On the other hand, the enantioresolution obtained on columns prepared through the single-step approach was quite unsatisfactory, and therefore the effect of using different linking spacers and crosslinkers was studied. A significant improvement of enantioresolution for 2-chloro-mandelic acid was obtained by using N , N -methylenebisacrylamide instead of ethylene dimethacrylate as the crosslinker in the single-step preparation.
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JOURNAL OF SEPARATION SCIENCE
·
2017
·Vol. 40
·期 7
·1548-1555
·
IF 2.557
Yufeng Zhou,Haijiao Zheng,Jiutong Ma,Qiong Jia
In the present study, a novel poly(acrylamide- co - N -isopropylacrylamide- co -ethylene dimethacrylate) monolithic column modified with saline-modified delaminated layered double hydroxides was developed and exploited as the stationary phase in the polymer monolith microextraction of β-agonists. Transmission electron microscopy, Fourier transform infrared spectroscopy, scanning electron microscopy, X-ray photoelectron spectroscopy, and thermal gravimetric analysis with derivative thermogravimetric determination were employed to characterize the monoliths. By coupling with high-performance liquid chromatography determinations, extraction parameters affecting the extraction efficiency, including sample volume, flow rate, sample pH, eluent volume, and eluent flow rate were investigated with an orthogonal experiment design, L 16 (4 5 ). Results demonstrated that under the optimal experimental conditions, low limits of detection in the range of 0.025–0.280 ng/mL were obtained with relative standard deviations in the range of 4.3–7.6% (intraday) and 6.7–8.8% (interday). When the developed method was applied to the analysis of β-agonists in pork samples, recovery values were obtained in the range of 80.5−108.6%.
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CHEMICAL RESEARCH IN CHINESE UNIVERSITIES
·
2016
·Vol. 32
·期 2
·172-177
·
IF 1.086
Song Shengmei,Ma Xuewen,Zhou Yehong,Xu Maotian,Shuang Shaomin,Dong Chuan
β -Amyloid(A β ) plaques and intracellular neurofibrillary lesions in the brain are markers of Alzheimer’s disease(AD). The ability to safely decrease A β concentrations is potentially important as a preventive strategy for AD. The interactions between vanillin and A β polypeptide were investigated via fluorescence spectroscopy and atomic force microscopy(AFM). The results of fluorescence and synchronous spectroscopies illustrate that the intrinsic fluorescence of tyrosine(Tyr) residues in A β
1-42 aggregates can be quenched strongly upon the formation of vanillin-A β
1-42 complex. Thioflavine T(ThT)-induced fluorescence changes indicated that A β
1-42 aggregates could be disaggregated by vanillin, and the AFM images of A β
1-42 enunciated the depolymerization of A β
1-42 aggregates by vanillin in a dose-dependent manner. Vanillin may be a potential pharmacological agent for the treatment of AD.
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2017
·
IF 2.603
Jingyi Zhang,Donghao Liu,Yi Shi,Chen Sun,Muchuan Niu,Ruya Wang,Fan Hu,Deli Xiao,Hua He
In this research, a novel insoluble sorbent based on cyclodextrin and rigid aromatic groups tetrafluoroacetonitrile was designed for dispersive insoluble solid-phase extraction (DSPE). Due to its high adsorption capacity, this obtained polymer was applied to separation and concentration of trace quinolones in wastewater before HPLC determination. Various parameters influencing the extraction performance were studied and optimized. A DSPE approach coupled with high performance liquid chromatography was developed for the determination of four quinolones in wastewater samples. The limit of quantitation of fleroxacin, ciprofloxacin, gatifloxacin, norfloxacin were 2.67, 3.17, 4.75, 5.50 ng mL −1 , respectively. The recoveries of four quinolones range from 96.43 to 103.3% with relative standard deviations less than 4.5%. These results demonstrated that the proposed approach based on CDP was efficient, low-cost for extraction of quinolones from wastewater.
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JOURNAL OF LUMINESCENCE
·
2016
·
IF 2.693
Chaolong Yang,Pan Zhang,Hualin Zhou,Jing Xu,Youbing Li,Mangeng Lu,Lei Lei,Qiang Zhang,Yi Zhang,Shaopeng Chen
A series of environment friendly Eu/PHB fluorescent films through doped the Eu-complex precursor Eu(TTA) 2 (Tpy-OCH 3 )(2H 2 O) into polymer matrices poly-β-hydroxybutyrate (PHB) with doping percentage at 1, 3, 5, and 7 (mass) were designed, fabricated and characterized. TGA and PL results indicated the Eu-complex precursor was immobilized in PHB matrix through the interaction between the Eu-complex. DSC results indicated the crystallinity of Eu/PHB films decreased with the increase of Eu-complex doping percentage. The emission spectra of the Eu-complex and Eu/PHB films recorded at room temperature exhibited the characteristic bands arising from the 5 D 0 / 7 F J . The fact that the quantum efficiencies ( η ) of the doped film increased significantly revealed that the PHB matrix acts as an efficient co-sensitizer for Eu 3+ ions luminescent center and therefore enhances the quantum efficiency of the emitter 5 D 0 level. In particular, all Eu/PHB films can be excited by visible light (410 nm), and also showed good photoluminescent properties. So the new Eu/PHB fluorescent films showed considerable promise for polymer light-emitting diode, active polymer optical fiber and biomedical analysis applications.
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Journal of Materials Chemistry B
·
2017
·Vol. 5
·期 42
·8330-8336
·
IF 4.543
Jing Han,Mengfei Zhang,Guojun Chen,Yongqing Zhang,Qing Wei,Ying Zhuo,Gang Xie,Ruo Yuan,Sanping Chen
Here a new type of ferrocene confined in a metal–organic framework (Fc-Zn-MOF) as an electrochemical signal tag has been synthesized and applied in an immunosensor for highly sensitive amyloid-β (Aβ, as a model protein) detection. In the present work, an electrochemically active molecule of Fc was covalently bonded in a Zn-MOF via postsynthetic modification to obtain a flower-like Fc-Zn-MOF, in which the high-content Fc signal units were periodically arranged in a well-defined porous structure, showing enhanced electrochemical activity. As noticed, Fc molecules are chemically anchored on the Zn-MOF, which avoids leakage of signal molecules, protects those electrochemical activities from potential damage and exhibits good stability. The Fc-Zn-MOF signal tag was further explored in constructing an electrochemical immunosensor for Aβ detection, with a linear range from 0.0001 to 100 ng mL−1 and a detection limit of 0.03 pg mL−1, showing improved analytical performance. This work presents an example of an Fc-MOF as a signal tag for Aβ detection, which would encourage atypical research lines for MOFs in bioassays where the introduction of ordered structures promises new opportunities.
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ANALYTICA CHIMICA ACTA
·
2017
·
IF 4.95
Haijiao Zheng,Tenggao Zhu,Xiqian Li,Jiutong Ma,Qiong Jia
A facile online method coupling polymer monolithic microextraction (PMME) with mass spectrometry (MS) was developed for the detection of Immunoglobulin G (IgG) galactosylation glycopeptides . A peanut agglutinin- β -cyclodextrin (PNA- β -CD) functionalized poly(hydroxyethyl methylacrylate-ethyleneglycol dimethacrylate) monolith was designed via a click reaction. Thanking to the specificity of PNA- β -CD for the targets, the material exhibited enhanced enrichment selectivity and extraction efficiency for IgG galactosylation glycopeptides. Under optimal conditions, the developed method gave a linear range of 0.005–5 pmol for IgG glycopeptides with the regression coefficient greater than 0.9990, and the detection limit of IgG galactosylation glycopeptides as low as 0.5 fmol was achieved. The PMME-MS method was applied to IgG galactosylation glycopeptides in real samples including human serum and acute myelogenous leukemia (AML) cell lysate. A series of unique IgG galactosylation glycopeptides were captured by the monolith in the complex samples, indicating satisfactory enrichment ability for IgG galactosylation glycopeptides. The quick and integrated online PMME-MS method exhibited high selectivity for IgG galactosylation, demonstrating its perspectives on the development and broad applications of MS in studying galactosylation proteins regulated biological processes .
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INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES
·
2017
·
IF 3.671
Ping Shao,Qiang Qiu,Jie Xiao,Yueqiong Zhu,Peilong Sun
The aim of the present study was to examine how factors (pH, temperature, iron chelators, and free radical scavengers) influence on the chemical stabilities of β-carotene encapsulated by Ulva fasciata polysaccharide (UFP)-stabilized emulsions and the bioaccessibility under in vitro oral-gastro-intestinal digestion conditions. The concentration of β-carotene in emulsions under different environments was determined. Changes in droplet properties, particle size and microstructure, throughout the oral-gastric-intestinal model were measured and the rate and extent of lipid digestion were recorded in the simulated small intestine fluid. Our results suggested that the pH had a significant effect on the stability of β-carotene, a rapid degradation at acidic environment and a relatively higher stability at high pH (6.0 and 7.0) were observed. β-carotene in emulsions was highly sensitive to extreme temperature (80 °C, 90 °C, and 100 °C). Addition of EDTA or α-tocopherol significantly increased the stability of β-carotene. Meanwhile, digested UFP-stabilized emulsions showed higher lipid digestion rate than GA-stabilized emulsions and BP-stabilized emulsions. UFP was capable of increasing the bioaccessibility of β-carotene in emulsions compared to GA and BP. Therefore, UFP-stabilized emulsion is a promising delivery system to promote applications of β-carotene in functional food and beverage system.
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