TALANTA
·
2015
·
IF 3.545
Qing Wang,Yao Long,Lin Yao,Li Xu,Zhi-Guo Shi,Lanying Xu
A mixed-mode chromatographic stationary phase , C18-DTT (dithiothreitol) silica (SiO 2 ) was prepared through “thiol-ene” click chemistry. The obtained material was characterized by fourier transform infrared spectroscope, nitrogen adsorption analysis and contact angle analysis. Chromatographic performance of the C18-DTT was systemically evaluated by studying the effect of acetonitrile content, pH, buffer concentration of the mobile phase and column temperature. It was demonstrated that the novel stationary phase possessed reversed phase liquid chromatography (RPLC)/hydrophilic interaction liquid chromatography (HILIC) mixed-mode property. The stop-flow test revealed that C18-DTT exhibited excellent compatibility with 100% aqueous mobile phase. Additionally, the stability and column-to-column reproducibility of the C18-DTT material were satisfactory, with relative standard deviations of retention factor of the tested analytes (verapamil, fenbufen , guanine , tetrandrine and nicotinic acid) in the range of 1.82–3.72% and 0.85–1.93%, respectively. Finally, the application of C18-DTT column was demonstrated in the separation of non-steroidal anti-inflammatory drugs, aromatic carboxylic acids , alkaloids, nucleo-analytes and polycyclic aromatic hydrocarbons . It had great resolving power in the analysis of various compounds in HILIC and RPLC chromatographic conditions and was a promising RPLC/HILIC mixed-mode stationary phase.
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TALANTA
·
2016
·
IF 4.035
Yating Xu,Ju Liu,Hongyang Zhang,Min Jiang,Lingling Cao,Min Zhang,Wei Sun,Shengli Ruan,Ping Hu
In this study, hypercrosslinked strong cation-exchange polymer resins (HXLPP-SCX) were synthesized and employed as selective sorbents for the solid-phase extraction (SPE) of basic purine metabolites associated with gout. The HXLPP-SCX material was prepared based on hypercrosslinking reactions and sulfonated with concentrated H 2 SO 4 . This synthetic procedure is facile and efficient without using highly toxic reagent. The resulting resins were characterized in the form of monodisperse microspheres (mean diameters of 3‒5 μm) with narrow pore size (2.1 nm) and relatively high specific surface areas (801 m 2 /g). The polymers also possess high ion-exchange capacity (IEC, 2.22 mmol/g) and good adsorption and selectivity performances for basic compounds. The resins used as SPE sorbents permit the selective enrichment of three pivotal purine metabolites (hypoxanthine, xanthine and inosine) in human serum followed by HPLC analysis. Method validation including linearity range, sensitivity, accuracy and reproducibility were evaluated. This method was exemplarily applied in the analysis of serum purines in gout patients and healthy controls. The present results demonstrate a promising potential of this HXLPP-SCX material for the clinical sample pretreatment.
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MICROCHIMICA ACTA
·
2014
·Vol. 182
·期 1
·185-192
·
IF 3.719
Wang Huiqi,Feng Wei,Jia Qiong
We show that graphene oxide functionalized with 3-aminophenylboronic acid represents a useful new adsorbent for the selective enrichment of the nucleosides, adenosine, guanosine, uridine, and inosine, which then were quantified by capillary electrophoresis. The analytes were separated within 10 min using a borate buffer of pH 9.3 (containing sodium dodecyl sulfate) at an operating voltage of 25 kV, a temperature of 20 °C, a sample injection time of 5 s, and with UV detection at 254 nm. The effects of sample pH, sample flow rate, eluent type, and eluent flow rate were optimized. Under the optimized conditions, the enrichment factor was determined to be 10. A linear relationship was obtained over the 0.1 to 100 μg mL −1 concentration range, with regression coefficients of >0.9991. The intra-day and inter-day relative standard deviations of this method were in the range of 3.1–5.0 % and 4.8–7.5 %, respectively. The method was applied to the determination of the nucleosides in (spiked) traditional Chinese medicine injection samples, and recoveries ranged from 70.8 to 106.7 %.
Graphene oxide functionalized with 3-aminophenylboronic acid was prepared for the enrichment of nucleosides combined with capillary electrophoresis. After optimizing various experimental parameters, the method was successfully applied to the determination of nucleosides in traditional Chinese medicine injection samples.
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NEW JOURNAL OF CHEMISTRY
·
2017
·Vol. 41
·期 15
·7133-7141
·
IF 3.269
Yue Hu,Wei Huang,Yukui Tong,Qinfei Xia,Miaomiao Tian
Boronate-affinity hollow molecularly imprinted polymers (h-MIPs) were prepared and applied to the selective enrichment of four nucleosides in traditional Chinese medicine injection samples, followed by HPLC detection. The synthesis mechanism of the h-MIPs was studied. Due to a large amount of boronic acid groups were introduced by 3-aminophenylboronic acid (APBA) in the outermost polymer shell of the MIPs, which was of great importance for improving the enrichment efficiency of the nucleosides. Furthermore, owing to the hollow structure of the h-MIPs, more binding cavities were located on the inner and outer surfaces of the h-MIPs, which could facilitate the removal of template molecules from the polymers and the rebinding of the target molecules to the polymers. Under optimal conditions, the detection limits of the four nucleosides were in the range of 0.012–0.033 μg mL−1. At the different spiked levels, the recoveries of the nucleosides were in the range of 63.8–108.9%. The proposed method was successfully applied to determine four nucleosides in five injection samples. The boronate-affinity h-MIPs provided a promising selective enrichment platform for precise nucleoside analysis.
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MICROCHIMICA ACTA
·
2017
·Vol. 184
·期 8
·2629-2636
·
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
·
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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PROCESS BIOCHEMISTRY
·
2016
·
IF 2.529
Yueqian Zhang,Junfen Wan,Xuejun Cao
Cordycepin is an antibiotic with excellent biological and pharmacological activities. In this work, surface imprinting technology was used for cordycepin purification. Gaussian 09 simulation software was used to screen out methacrylic acid and acrylamide as the functional monomers of molecularly imprinted polymers (MIPs). The synthesis was accomplished with modified silica gel as a matrix, cordycepin as a template, methacrylic acid and acrylamide as functional monomers, ethyleneglycol dimethacrylate as a crosslinking agent and azodiisobutyronitrile as an initiator. MIPs for cordycepin separation were characterized by scanning electron microscope, Fourier transform infrared spectroscopy, elemental analysis and the pore size distribution analysis method. Adsorption isotherms for cordycepin show that the adsorption capacity using an initial cordycepin concentration of 16 mg/mL was 91.78 mg/g. According to the adsorption kinetic curve, MIPs obtained the maximum adsorption amount at 95.37 mg/g. In the adsorption kinetic experiments, adsorption reached equilibrium at 14 h with a rapid increase up to 4–6 h. The selectivity coefficients of MIPs were 3.14 (cordycepin versus inosine) and 3.74 (cordycepin versus adenosine). Experimental results indicated that the adsorption capacity and selectivity of MIPs were sufficient for the separation of cordycepin. MIPs were used to separate cordycepin from Cordyceps militaris . Cordycepin with 98% purity was obtained with the recovery of 25.67%. This result showed that MIPs prepared in this method have a good application prospect in the separation of cordycepin.
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BIOMEDICAL CHROMATOGRAPHY
·
2016
·Vol. 31
·期 4
·e3860
·
IF 1.729
Yan Du,Yin-jie Li,Xun-xiu Hu,Xu Deng,Zeng-ting Qian,Zheng Li,Meng-zhe Guo,Dao-quan Tang
As essential endogenous compounds, nucleobases and nucleosides fulfill various functions in living organisms. This study presents the development and validation of a new hydrophilic interaction liquid chromatography tandem mass spectrometry method for simultaneous quantification of 19 nucleobases and nucleosides in rat plasma. For the sample preparation, 15 kinds of protein precipitants were evaluated according to the chromatographic profile and ion response of analytes. The optimization of chromatographic separation was respectively performed using reversed-phase liquid chromatography and hydrophilic interaction liquid chromatography mode; each separation mode included two test columns with different stationary phases. The chromatographic profile and parameters such as half-width ( W 1/2 ), capacity factor ( K ′) and tailing factor ( f t ) were used to evaluate the separation efficiencies. Furthermore, the adopted composition of two mobile phase systems and the concentrations of the additives in the optimum buffer system were also investigated. The developed method was fully validated and successfully applied quantitatively to determine 19 nucleobases and nucleosides in plasma from normal and diabetic nephropathy (DN) rats. Significant differences between normal and DN rats were found in plasma levels of cytosine, xanthine, thymidine, adenosine, guanosine, inosine and 8-hydroxy-2′-deoxyguanosine. This information may provide a useful reference for the discovery of potential biomarkers of DN.
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JOURNAL OF CHROMATOGRAPHY A
·
2016
·
IF 3.926
Haibin Li,Chusheng Liu,Qiqin Wang,Haibo Zhou,Zhengjin Jiang
In order to investigate the effect of charged groups present in hydrophilic monolithic stationary phases on their chromatographic properties, three charged hydrophilic monomers, i.e. N,N -dimethyl- N -acryloyloxyethyl- N -(3-sulfopropyl)ammonium betaine (SPDA), [2-(acryloyloxy)ethyl]trimethylammonium chloride (AETA), and 3-sulfopropyl acrylate potassium salt (SPA) were co-polymerized with the crosslinker N,N '-methylenebisacrylamide (MBA), respectively. The physicochemical properties of the three resulting charged hydrophilic monolithic columns were evaluated using scanning electron microscopy, ζ-potential analysis and micro-HPLC. High column efficiency was obtained on the three monolithic columns at a linear velocity of 1 mm/s using thiourea as test compound. Comparative characterization of the three charged HILIC phases was then carried out using a set of model compounds, including nucleobases, nucleosides, benzoic acid derivatives, phenols, β-blockers and small peptides. Depending on the combination of stationary phase/mobile phase/solute, both hydrophilic interaction and other potential secondary interactions, including electrostatic interaction, hydrogen-bonding interaction, molecular shape selectivity, could contribute to the over-all retention of the analytes. Because of the strong electrostatic interaction provided by the quaternary ammonium groups in the poly (AETA- co -MBA) monolith, this cationic HILIC monolith exhibited the strongest retention for benzoic acid derivatives and small peptides with distorted peak shapes and the weakest retention for basic β-blockers. The sulfonyl groups on the poly (SPA- co -MBA) hydrophilic monolith could provide strong electrostatic attraction and hydrogen bonding for positively charged analytes and hydrogen-donor/acceptor containing analytes, respectively. Therefore, basic drugs, nucleobases and nucleotides exhibited the strongest retention on this anionic monolith. Because of the weak but distinct cation exchange properties of the zwitterionic poly (SPDA- co -MBA) hydrophilic monolith, it exhibited the best separation for most test analytes (including phenols, β-blockers and small peptides) in terms of selectivity, peak shape and analysis time. The poly (AETA- co -MBA) hydrophilic monolithic column provides the best separation of nucleobases and nucleosides. These results could guide the selection and application of these charged HILIC monoliths in the future.
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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
·
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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