MICROCHIMICA ACTA
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2017
·Vol. 184
·期 8
·2629-2636
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IF 4.58
Cai Tianpei,Zhang Haijuan,Rahman A. F. M. Mustafizur,Shi Yan-Ping,Qiu Hongdeng
Carbon dots derivatized from N-(β-aminoethyl)-γ-aminopropyl-methyldimethoxysilane (AEAPMS) were coated onto silica microparticles. These particles (Sil-CDs) are shown to be an excellent stationary phase for use in hydrophilic interaction chromatography. Analytes including sulfonamides, nucleosides and bases, flavones and amino acids can be well separated on this stationary phase. Compared to a silica stationary phase functionalized with AEAPMS only, the Sil-CDs show enhanced separation performance. The selectivity factors of three nucleosides and bases (1.02–1.09) and four sulfonamides (1.04–1.11) on AEAPMS functionalized silica stationary phase were improved to 1.10–1.20 and 1.13–1.15 respectively on Sil-CDs stationary phase. This is attributed to the higher number of surface functional groups due to the introduction of carbon dots. The successful application of the Sil-CDs stationary phase highlights the potential of carbon dots as a modified material in chromatography.
Schematic presentation of the preparation of silanized carbon dots coated onto silica microparticles. The material represents a new stationary phase for hydrophilic interaction chromatography. It shows improved separation performance compared to a silane-only functionalized silica stationary phase.
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JOURNAL OF SEPARATION SCIENCE
·
2016
·Vol. 39
·期 7
·1347-1356
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IF 2.741
Ting Cheng,Shuqiang Zhu,Bin Zhu,Xiaoyan Liu,Haixia Zhang
The nucleoside or modified nucleoside level in biological fluids reflects the pathological or physiological state of the body. Boronate affinity absorbents are widely used to selectively extract nucleosides from complex samples. In this work, a novel functionalized absorbent was synthesized by attaching 4-mercaptophenylboronic acid to gold nanoparticles on modified attapulgite. The surface of the attapulgite was modified by poly(acryloyloxyethyltrimethyl ammonium chloride) by atom transfer radical polymerization, creating many polymer brushes on the surface. The resultant material exhibited superior binding capacity (30.83 mg/g) for adenosine and was able to capture cis -diol nucleosides from 1000-fold interferences. Finally, to demonstrate its potential for biomolecule extraction, this boronate affinity material was used to preconcentrate nucleosides from human urine and plasma.
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TALANTA
·
2016
·
IF 4.035
Huihui Li,Ting Cheng,Shuxia Wang,Xinyue Zhu,Haixia Zhang
Boronate affinity materials have been widely used for selective capture of cis-diol-containing molecules, but most do not have sufficient extraction efficiency. We have prepared boronic acid-functionalized attapulgite, and then it was coated with imidazolium-based ionic liquid , 1-dodecyl-3-methylimidazolium bromide (C 12 mimBr), via physical self-assembly process. The extraction efficiency of the material increased dramatically after coated with C 12 mimBr, and its enrichment ratios for nucleosides increased by 9- to 282-fold. Besides, the C 12 mimBr-coated adsorbent did not lose selectivity and was able to capture cis-diols in the presence of a 100-fold excess of interferences. C 12 mimBr-coated material was applied to selective enrichment of nucleosides from human urine. The limits of detection and the limits of quantification were in the range of 0.06–0.46 ng mL −1 and 0.20–1.53 ng mL −1 , respectively. Reproducibility of the method was determined with relative standard deviations≤9.9%. The recoveries of the target nucleosides from spiked human urine were in the range of 87.8–109.6%. In our preception, self-assembly ionic liquid layer can serve as a promising alternative to improve the extraction efficiency of boronate affinity materials.
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JOURNAL OF CHROMATOGRAPHY A
·
2017
·
IF 3.981
Chusheng Liu,Haibin Li,Qiqin Wang,Jacques Crommen,Haibo Zhou,Zhengjin Jiang
The quest for higher column efficiency is one of the major research areas in polymer-based monolithic column fabrication. In this research, two novel polymer-based HILIC monolithic columns with 400 μm I.D. × 800 μm O.D. were prepared based on the thermally initiated co-polymerization of N,N -dimethyl- N -(3-methacrylamidopropyl)- N -(3-sulfopropyl) ammonium betaine (SPP) and ethylene glycol dimethacrylate (EDMA) or N,N’ -methylenebisacrylamide (MBA). In order to obtain a satisfactory performance in terms of column permeability, mechanical stability, efficiency and selectivity, the polymerization parameters were systematically optimized. Column efficiencies as high as 142, 000 plates/m and 120, 000 plates/m were observed for the analysis of neutral compounds at 0.6 mm/s on the poly(SPP- co -MBA) and poly(SPP- co -EDMA) monoliths, respectively. Furthermore, the Van Deemter plots for thiourea on the two monoliths were compared with that on a commercial silica based ZIC-HILIC column (3.5 μm, 200 Å, 150 mm × 300 μm I.D.) using ACN/H 2 O (90/10, v/v) as the mobile phase at room temperature. It was noticeable that the Van Deemter curves for both monoliths, particularly the poly(SPP- co -MBA) monolith, are significantly flatter than that obtained for the ZIC-HILIC column, which indicates that in spite of their larger internal diameters, they yield better overall efficiency, with less peak dispersion, across a much wider range of usable linear velocities. A clearly better separation performance was also observed for nucleobases, nucleosides, nucleotides and small peptides on the poly(SPP- co -MBA) monolith compared to the ZIC-HILIC column. It is particularly worth mentioning that these 400 μm I.D. polymer-based HILIC monolithic columns exhibit enhanced mechanical strength owing to the thicker capillary wall of the fused-silica capillaries.
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JOURNAL OF CHROMATOGRAPHY A
·
2016
·
IF 3.926
Jialiang Guo,Yuan Xiao,Yuanjing Lin,Jacques Crommen,Zhengjin Jiang
Low column efficiency for enantioseparations in capillary liquid chromatography (CLC) is a major problem commonly encountered with β -cyclodextrin ( β -CD) functionalized polymer-based monoliths. In order to investigate the effect of the crosslinker type on enantioseparation performance, three commonly used crosslinkers, i.e. 1,4-bis(acryloyl)piperazine (PDA), ethylene dimethacrylate (EDMA) and N , N -methylenebisacrylamide (MBA), were copolymerized using the one-pot approach with glycidyl methacrylate-mono-6-amino-6-deoxy- β -CD (GMA-NH 2 - β -CD) as functional monomer. The three monolithic columns, including poly(GMA-NH 2 - β -CD- co -PDA) and poly(GMA-NH 2 - β -CD- co -MBA), as well as the previously reported column poly(GMA-NH 2 - β -CD- co -EDMA) were systematically compared with respect to morphology, permeability, β -CD density, retention mechanism and efficiency. The enantioseparation ability of each column was evaluated using 14 chiral compounds, including mandelic acid derivatives, profens, N -derivatized amino acids, and herbicides, as test substances. The β -CD-functionalized monolith with MBA as crosslinker was found to exhibit higher polarity, higher column efficiency and better enantioseparation performance than those with PDA or EDMA as crosslinker.
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TALANTA
·
2017
·
IF 4.162
Shuxia Wang,Huihui Li,Xiujuan Guan,Ting Cheng,Haixia Zhang
Boronic acid modified materials have been widely used to adsorb nucleosides , but their adsorption capacities require further improvement. Most cis -diol containing biomolecules are in very low abundance along with interfering components in real samples, and need to be enriched specially. In this study, we synthesize a kind of silica absorbent modified with boronic acid derivative, using amorphous silica as raw material and obtaining high adsorption capacity for adenosine. In addition, the adsorption equilibrium can be completed within 10 s and 1 min for the desorption. Finally, the material was successfully applied to enrich nucleosides from cells and the spiked recoveries were found between 82.21% and 118.9%. The results showed that the prepared adsorbent has potential to effectively enrich cis-diol substances from cell samples.
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JOURNAL OF CHROMATOGRAPHY A
·
2017
·
IF 3.981
Chen Zhao,Yan Yang,Linfang Wei,Qinghua Guo,Hao Fang,Shaolin Chen,Qiang Hua
Yarrowia lipolytica is an oleaginous yeast with promise in producing terpenoids such as lycopene . Though methods for analyzing primary metabolic intermediates have been established, further work is needed to better analyze nucleotides and coenzymes . Here, we presented an optimized method for the separation of nucleotides and coenzymes in Y. lipolytica using the capillary electrophoresis. The separation of twelve metabolites including four coenzymes, five nucleotides and three nucleosides was achieved within 32 min using a voltage of 15 kV and 70 mM sodium carbonate/hydrogencarbonate buffer with 1.0% β -CD at pH 10. The results show that the concentrations of adenosine triphosphate and nicotinamide adenine dinucleotide phosphate changed significantly between lycopene producing strain and the control, indicating that these two metabolites may be closely related with lycopene production. The optimized method provides a useful approach for future metabolic analysis of fermentation process as well as industrial strain improvement.
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2017
·
IF 3.255
Yang Huang,Tingting Zhang,Yumei Zhao,Haibo Zhou,Guangyun Tang,Marianne Fillet,Jacques Crommen,Zhengjin Jiang
Nucleobases, nucleosides and ginsenosides, which have a significant impact on the physiological activity of organisms, are reported to be the active components of ginseng, while they are less present in ginseng extracts. Few analytical methods have been developed so far to simultaneously analyze these three classes of compounds with different polarities present in ginseng extracts. In the present study, a simple and efficient analytical method was successfully developed for the simultaneous separation of 17 nucleobases, nucleosides and ginsenosides in ginseng extracts using supercritical fluid chromatography coupled with single quadrupole mass spectrometry (SFC-MS). The effect of various experimental factors on the separation performance, such as the column type, temperature and backpressure, the type of modifier and additive, and the concentration of make-up solvent were systematically investigated. Under the selected conditions, the developed method was successfully applied to the quality evaluation of 14 batches of ginseng extracts from different origins. The results obtained for the different batches indicate that this method could be employed for the quality assessment of ginseng extracts.
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NEW JOURNAL OF CHEMISTRY
·
2018
·Vol. 42
·期 7
·4909-4914
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IF 3.201
Yuanyuan Xu,Yue Yang,Aifang Xue,Hao Chen,Shengqing Li
Pure titanium dioxide (TiO2) adsorbent failed to selectively capture ribonucleosides in biological samples, as reported in previous studies, although it was expected to display a specific recognition of cis-diol compounds by the Lewis acid sites on its surface. However, in this work, our results showed for the first time that hydrous titania (TiO2·nH2O), obtained through hydrolysis of tetrabutyl titanate (TBOT) in aqueous solution, exhibited a high affinity for cis-diol-containing ribonucleosides. The adsorption efficiency of A, C and G by TiO2·nH2O can reach about 90% even in a 100% water matrix. On the other hand, the 2′-deoxynucleosides could only be adsorbed in a water–acetonitrile solution with a water content of less than 10%. Subsequently, an in situ-generated TiO2·nH2O-based dispersive micro solid-phase extraction (d-μ-SPE) process was developed and evaluated. The whole d-μ-SPE process takes only about 7 minutes (2 min for extraction and 5 min for centrifugation) and no pre-synthesized or commercial TiO2 powder is required. The hydrous TiO2-based d-μ-SPE with a two-step elution strategy was successfully performed for the extraction and separation of ribonucleosides (A, U) and 2′-deoxynucleosides (2′-dC, 2′-dG) in porcine plasma samples. The proposed TiO2·nH2O-based d-μ-SPE method is effective, simple and rapid, and will have wide application for the selective extraction of cis-diol molecules in environmental and biological samples.
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MICROCHIMICA ACTA
·
2017
·Vol. 185
·期 1
·1-9
·
IF 4.58
Hu Yue,Xia Qinfei,Huang Wei,Hou Xingyu,Tian Miaomiao
D-Glucose was used as a dummy template in a strategy to fabricate boronate-based hollow molecularly imprinted polymers (h-MIPs) for the recognition of glycosides. 3-Aminophenylboronic acid (APBA) was selected as the functional monomer to impart glycoside binding capability. A polystyrene core was synthesized via an emulsifier-free emulsion polymerization. It was then be corroded to form a hollow structure where the binding sites on the inner surface can be fully utilized. Adsorption studies indicate that the resulting h-MIPs can specifically recognize glycosides. The h-MIPs were applied as a sorbent for solid phase extraction of the glycosides (daidzin, glycitin, rutin, and genistin) in soy products. Following desorption with 1% TFA in acetonitrile-water (3:7, v / v ), the glycosides were quantified by HPLC with UV detection. The detection limits for the glycosides range from 3.5 to 10.8 ng·mL −1 .
Boronate-affinity hollow molecularly imprinted polymers using D-glucose as dummy template were prepared as solid phase extraction adsorbents for selective enrichment of glycosides in soy products prior to quantitation by HPLC-UV.
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SENSORS AND ACTUATORS B-CHEMICAL
·
2017
·
IF 5.401
Wanying Zhu,Xin Shen,Chunhong Zhu,Bingzhi Li,Junli Hong,Xuemin Zhou
In this work, based on purifying the analysis system by magnetic separation, we constructed a turn-on fluorescent assay for highly sensitive detection of possible biomarkers, employing adenosine as the model target analyte. Aptamer labeled-carbon dots (Apt-CDs) was applied as fluorescence probes as well as selective recognition elements, while Fe 3 O 4 @polypyrrole (Fe 3 O 4 @PPY) was used as fluorescence quenching and magnetic separating materials for system purification. In absence of adenosine, the Apt-CDs were attached to the surface of PPY through π-π stacking and hydrophobic interaction and its fluorescence was quenched by Fe 3 O 4 @PPY. In presence of adenosine, the aptamer could specifically bind with adenosine to form a three dimensional Apt-CDs-adenosine complex and detach from PPY, leading to the fluorescence recovery of Apt-CDs. More importantly, with analysis system purification via twice convenient magnetic separations of free CDs and Apt-CDs-adenosine complex respectively, the detection limit could be reduced from 8 nmol L −1 to 0.15 nmol L −1 . This concept offers potential application for simple, rapid, cost-effective, and highly sensitive assay of biological samples.
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NEW JOURNAL OF CHEMISTRY
·
2018
·Vol. 42
·期 3
·2288-2294
·
IF 3.201
Yanan Pan,Xiumei Guo,Shanshan Li,Xiaoyan Liu,Haixia Zhang
In this study, a new boronate affinity porous carbon absorbent derived from a home-made zinc-based metal–organic framework (Zn-MOF) was successfully fabricated. This absorbent was prepared by calcination of the Zn-MOF material and further modified with boronic acid groups. The resulting material was used to selectively enrich cis-diol-containing nucleosides in complex samples, and it exhibited superior binding capacity (26.0 mg g−1 for adenosine). The material coupled with high-performance liquid chromatography was successfully applied to analyze four cis-diol nucleosides (cytidine, uridine, guanosine, and adenosine) in injection and cell samples. Under optimized conditions, the method exhibited excellent extraction performance. The limits of detection of the method were 4.73–14.6 μg L−1 for the four nucleosides based on the signal-to-noise ratio of 3 : 1. Spiked recoveries were found between 88.2 and 108.2% (the relative standard deviation was in range of 1.3–11.3%, n = 3). This study improved the selectivity of porous carbon derived from MOF material and presented a promising thought for effective capturing of analytes on MOF materials.
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