BIOMEDICAL CHROMATOGRAPHY
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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 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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JOURNAL OF CHROMATOGRAPHY A
·
2025
·
IF 4
Liang Lai,Hongying Lan,Hui Huang,Tong Li,Kesara Ar-sanork,Jia-Huan Qu,Dongsheng Xu,Zhengjin Jiang
In this study, the chromatographic performance of a novel dual-zwitterionic hydrophilic stationary phase were investigated. Three zwitterionic HILIC monoliths were prepared using 3-(4-((methacryloyloxy)methyl)-1-methylpiperidin-1-ium-1-yl)propane-1-sulfonate (MAMMPS), 2-methacryloyloxyethyl phosphorylcholine (MPC), and a combination of MAMMPS and MPC (1:1, molar ratio) with N,N' -methylenebisacrylamide (MBA), separately. The monoliths exhibited good repeatability and stability. A high column efficiency of 120,000 plates/m was reached on the novel dual-zwitterionic functionalized poly(MAMMPS@MPC- co -MBA) monolith. Through the analysis and testing with different standards, the poly(MAMMPS@MPC- co -MBA) monolith exhibited the strongest retention capacity for negatively charged benzoic acid derivatives due to its high hydrophilicity and weak electronegativity. In contrast, the poly(MPC- co -MBA) monolith, functionalized with a single zwitterion, facilitated electrostatic interactions with negatively charged analytes. Baseline separation was achieved on all three monoliths for selected nucleobases, nucleosides, phenol derivatives, and amine compounds. However, their retention strength was mainly related to the hydrophilicity of the stationary phases, while hydrogen bonding and electrostatic interactions played secondary roles. Among the monoliths, the poly(MAMMPS- co -MBA) monolith demonstrated the best separation for neutral, acidic, and alkaline compounds. These findings offer valuable insights for the future selection and application of dual-zwitterionic HILIC monoliths for chromatographic separations.
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Journal of Analysis and Testing
·
2025
·
IF 7
Li Han,Cui Yuanyuan,Zhen Changqing,Lin Xiaohui,Li Ke,Yang Chengxiong
Microporous organic network (MON) has emerged as efficient stationary phases for high-performance liquid chromatographic (HPLC) separation. Nevertheless, the inherent superhydrophobic networks made their applications limited in the reversed-phase (RP) mode. In this work, a novel amino acid L-cysteine (L-Cys) modified core-shelled microsphere MON@SiO 2 -L-Cys was synthesized via the efficient thiol-yne “click” reaction for hydrophilic interaction chromatography /reversed-phase liquid chromatography (HILIC/RPLC) mixed-mode chromatographic separation. Baseline separation of various hydrophilic and hydrophobic compounds including aromatic ketones, phthalate esters, alkylbenzenes, amines, polycyclic aromatic hydrocarbons, phenols, nucleosides, nucleic acid bases, sulfonamides, water-soluble vitamins, cephalosporin antibiotics, and estrogens was realized on MON@SiO 2 -L-Cys packed column based on the predesigned mixed-mode retention mechanisms. The MON@SiO 2 -L-Cys packed column also exhibited higher selectivity compared to bare SiO 2 , MON@SiO 2 without L-Cys, and C 18 packed columns, revealing the synergistic interactions of MON’s networks and the modified L-Cys molecules. This work provided a feasible way to construct a novel amphipathic MON-based stationary phase, broadened the application scope of MON for hydrophilic analytes, and uncovered the prospects of MON in mixed-mode HPLC.
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NEW JOURNAL OF CHEMISTRY
·
2018
·Vol. 42
·期 7
·4909-4914
·
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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ANALYTICAL CHEMISTRY
·
2018
·
IF 6.042
Mengzhe Guo,Liyan Zhang,Yan Du,Wencheng Du,Dantong Liu,Cheng Guo,Yuanjiang Pan,Daoquan Tang
5-(Hydroxymethyl)-2′-deoxycytidine (5-hmdC), 5-(formyl)-2′-deoxycytidine (5-fodC), and 5-(carboxyl)-2′-deoxycytidine (5-cadC) are crucial intermediate products of the DNA demethylation pathway, which can also act as potential biomarkers reflecting the diagnosis and prognosis in multiple tumors. Detecting 5-hmdC, 5-fodC, and 5-cadC in human urine has various advantages including readily available samples and being noninvasive to patients. However, few works have reported the detection of 5-fodC and 5-cadC due to their trace amounts. Here we developed a novel magnetic hyper-cross-linked microporous polymer (HMP) material based on polyionic liquid (PIL) for the enrichment of 5-hmdC, 5-fodC, and 5-cadC. These magnetic PIL-HMP materials provided specific enrichment superiority for three modified cytidines. After enrichment, the signal intensity of 5-hmdC, 5-fodC, and 5-cadC increased 10–75-fold with lower limits of quantitation (LLOQ) of 0.049, 0.781, and 0.781 ng/mL, respectively. The recoveries were approximately 86.5–95.2% for 5-hmdC, 95.2–107.8% for 5-fodC, and 99.4–102.4% for 5-cadC under the relative standard deviation (RSD) of 0.2–10.3%. Finally, we successfully applied magnetic PIL-HMP materials coupled with high-performance liquid chromatography–electrospray ionization tandem mass spectrometry (HPLC-ESI-MS/MS) in enrichment and quantitative determination of 5-hmdC, 5-fodC, and 5-cadC in human urine of 10 breast cancer patients and 10 healthy people. We found that the level of 5-hmdC decreased in breast cancer patients (p < 0.05), while the levels of 5-fodC and 5-cadC increased (p < 0.05, p < 0.01). Our results demonstrated that the levels of metabolic 5-hmdC, 5-fodC, and 5-cadC in human urine are closely related to breast cancer, which could contribute to the clinical diagnosis and investigation of breast cancer and its occurrence and development mechanisms.
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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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SENSORS AND ACTUATORS B-CHEMICAL
·
2025
·
IF 7.7
Mengzhen Jiang,Ruohan Xu,Chunyan Yang,Haili Wang,Jinyuan Cai,Yanrong Wen,Mingfu Ye,Tingxuan Yan,Shuangshou Wang
cis -Diol compounds are of great biological and clinical values, but their detection is usually instrument-inseparable. Herein, a flexible sensing strategy was proposed at the first time for multi-mode visualization of cis -diol compounds based on boronate affinity (BA)-mediated colorimetry and fluorometry. Boronic acid-decorated sensors with color-/fluorescence-derived binary responsivity were designed using cis -diol fluorescent dyes or dyes-fluorophore counterparts as response units, inducing competitive BA when cis -diol analytes were existed. Consequently, colors and fluorescence of sensors changed simultaneously, and both signals were linearly varied versus the dosages of cis -diol analytes in certain ranges. As proofs of concept, dual-mode visual sensing of glucose in normal/hyperglycemic human serum and sucrose in canned white fungus and edible mushroom plant beverage was achieved with sensing time as short as 1 min and limit of detection as low as 0.18 mg/mL. Furtherly, color information of colorimetric/fluorometric cards and tested sensors was picked by a smartphone APP for digital image analysis, by which the validity of dual-mode visual sensing assays was reinforced by avoiding possible errors from subjective judgement on colors and fluorescence. Besides, the credibility of visual sensing was cross-validated by fluorescent quantification and classical tools such as portable blood glucose meter and phenol-sulfuric acid method-based halochromic reaction.
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TALANTA
·
2011
·
IF 3.722
Junxia Hao,Fuqiang Wang,Xiaojun Dai,Bolin Gong,Yinmao Wei
A novel stationary phase for weak cation exchange (WCX) and hydrophilic interaction chromatography (HILIC) was prepared with surface-initiated atom transfer radical polymerization (SI-ATRP). Vinyltetrazole was grafted onto the surface of the beads in water medium with the polyglycidylmethacrylate beads (P GMA/EDMA ) previously modified with 2-bromoisobutryl bromide as the macromolecule initiators and CuCl as catalyst. The poly(vinyltetrazole)-grafted beads obtained with different atom transfer radical polymerization (ATRP) formulations were tried as chromatographic packings in ion-exchange chromatography. The results showed that the prepared columns could separate the tested proteins with high efficiency and high capacity, and the retention time of protein had a positive relationship with increasing the chain lengths of the grafted poly(vinyltetrazole) (PVT). The prepared column was also found to be able to separate nucleosides by hydrophilic interaction chromatographic mode.
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