NEW JOURNAL OF CHEMISTRY
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2020
·Vol. 44
·期 27
·11704-11709
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IF 3.288
Chao Fan,Hao Tang,Licheng Wang,Yijing Li,Xusheng Wang,Shuai Wang,Xiaojing Liang
Using N-isopropylacrylamide (NIPAM) as a monomer, a core–shell material was successfully prepared via in situ polymerization on the surface of silica microspheres (named NIPAM@Sil), which acts as a hydrophilic interaction chromatography (HILIC) stationary phase. A method for the in situ polymerization of polymer monomers on a silica surface has been developed. It was shown using scanning electron microscopy (SEM) that NIPAM is evenly distributed on the surface of the silica. The synthesized NIPAM@Sil possesses a polar acylamino group arising from the polymerization of NIPAM. As demonstrated by the hydrophilicity, NIPAM@Sil showed excellent HILIC performance for the separation of hydrophilic compounds. This method provides a simple approach for the preparation of a polymer coated silica core–shell stationary phase.
研究领域:
分析化学
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材料科学
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高影响因子
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.
研究领域:
分析化学
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色谱技术
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PubMed
高影响因子
International Journal of Analytical Chemistry
·
2015
·
IF 1
Yahui Ge,Yuping Tang,Sheng Guo,Xin Liu,Zhenhua Zhu,Pei Liu,Jin-ao Duan
Thais clavigera, as function food, is distributed widely along the coasts of China. To compare and tap its potentially nutritional and functional values, hydrophilic interaction ultra-performance liquid chromatography coupled with triplequadrupole tandem mass spectrometry (HILIC-UPLC-TQ-MS/MS) was used for simultaneous identification and quantification of amino acids, nucleosides, and nucleobases in the extracts of T. clavigera from 19 sea areas in China, and a PCA was further performed for comparing their content variation in different distribution regions. The total contents of amino acids varied from 116.74 mg/g to 298.58 mg/g being higher than contents of nucleosides and nucleobases that varied from 2.65 mg/g and 20.49 mg/g. Among the habitats, Hainan province had content advantages on others. By PCA, samples collected from different regions were classified into three groups. For specific constituents, lysine accounted for large part of essential amino acids; glycine and taurine also play important roles in the delicate taste and health care function of it. Inosine takes up most of total contents of nucleosides and nucleobases. These results provided good data for establishing quality standard of T. clavigera related products and their further development and utilization.
研究领域:
海洋生物学
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营养学
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分析化学
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PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2025
·
IF 4
Minyi Yuan,Zheng Zhao,Ji Wu,Sumin Bian,Yuling Liao,Ying Zhou,Huikai Shao,Zhengjin Jiang,Qiqin Wang
To meet the increasing demand for the separation of complex samples, a novel monolithic stationary phase with hydrophobic and hydrophilic functionalities was developed by using 3-(1-(4-vinylbenzyl)-1H-imidazol-3-ium) propane-1-sulfonate (VBIPS) as monomer, pentaerythritol triacrylate (PETA) as crosslinker. The optimized mixed-mode poly(VBIPS- co -PETA) monolith exhibited good mechanical strength, high permeability (K = 0.23 × 10 -14 m 2 in 100% ACN, 0.23 × 10 -14 m 2 in 100% MeOH, and 0.11 × 10 -14 m 2 in 100% H 2 O), and multiple interaction modes, including hydrophilic, hydrophobic, hydrogen, and electrostatic interactions. The highest column efficiency of 83,330 plates/m was achieved for thiourea at a linear velocity of 0.23 mm/s. Systematic evaluations confirmed strong retention and separation of polar substances (e.g., benzoic acids, nucleoside bases, phenols), primarily due to the sulfobetaine-derived hydrophilicity as well as effective separation of nonpolar substances (e.g., aniline, aryl ketones, polyaromatic hydroxy compounds), facilitated by π-π stacking interactions between analytes and benzene rings within the stationary phase. Overall, this zwitterionic imidazolium sulfonate-functionalized monolith successfully combines hydrophobic and hydrophilic groups in a single continuous bed, enabling efficient separation of both polar and nonpolar analytes under low backpressure. This work enriches the library of mixed-mode stationary phases, and broadens the detection scope for complex sample analysis.
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高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2019
·
IF 2.983
Yong-Gang Xia,Si-Miao Yu,Jun Liang,Bing-You Yang,Hai-Xue Kuang
A generic strategy based on chemical fingerprinting is proposed for the differentiation of polysaccharides from Astragalus membranaceus (AEP) and A. mongholicus (AOP), using multiple chromatographic and mass spectrometric techniques. Complete and mild acid hydrolysis and Smith degradation were employed for the depolymerization of polysaccharides. The corresponding digested products were efficiently separated and detected using GC–MS, HILIC-ELSD and HR-ESI − -MS. The resulting bottom-up fingerprinting reflected the variations in native polysaccharides, which may be attributed to the three structural levels, which are monosaccharide compositions, glycosidic linkages, and skeletal structure. Similarity analysis from GC–MS and HILIC-ELSD fingerprinting showed that the correlation coefficients from homologous species were more than 0.914, whereas those from heterologous species were less than 0.796. It also noted that characteristic peak area ratio of Man/Gal in Smith fingerprinting could be used a feasible parameter for direct discrimination of AEP and AOP. Principal component analysis from m/z fingerprinting data resulted in clear clustering of AEP and AOP based on changes of oligosaccharides in mild acid hydrolyzates. By combining the accurate m/z , ESI − -MS/MS and methylation assays, the structures of a series of hexose glycopolymers in mild acid hydrolyzates were characterized by predominant 1,6 glycosidic linkages along with minor 1,4 glycosidic linkages. The established chemical fingerprinting is not only an interconnected structure mapping but also a powerful approach for the evaluation of polysaccharides from traditional Chinese medicines.
研究领域:
中药学
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分析化学
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PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2018
·
IF 3.716
Guozhu Liu,Baolei Luan,Guiting Liang,Libo Xing,Liang Huang,Changyun Wang,Ying Xu
Capreomycin has good clinical utility to treat multidrug resistant tuberculosis, but it is only used as a second line drug due to its adverse reactions. Literature has demonstrated that the toxicity of capreomycin product is significantly influenced by the impurities in it. Unfortunately, so far, no one impurity in capreomycin has ever been isolated and definitely identified due to its extremely strong basic character and high polarity. An ion-pair method reported in literature can provide separation of capreomycin and its impurities, but it is hard to be used for the preparative purpose. In this study, this ion-pair method was further improved to detect more impurities in capreomycin sulfate substance. Besides the four main components (IA, IB, IIA and IIB), four impurities (impurity A–D) with their contents much higher than the identification threshold were observed. Furthermore, a two dimensional (2D) LC quadrupole-time of flight (Q-TOF) MS method was established to realize high resolution MS analysis of these impurities. For the purpose of preparative isolation, a hydrophilic interaction chromatography (HILIC) method was established. The four main components were well isolated, but unfortunately, the four impurities were co-eluted with each other or with IB by the HILIC method. Fortunately, the degradation experiments revealed that IA and IB could yield clean impurity A and B respectively in acidic medium, and can yield clean impurity D and C respectively in alkaline medium. Therefore, IA and IB were first isolated by the preparative HILIC method, then pure IA and IB underwent acid degradation and base degradation separately and followed by re-isolation by the HILIC method to obtain pure impurity A–D respectively. Based on Q-TOF MS and NMR analysis, the structures (including absolute configuration) of the four isolated impurities were definitely identified.
研究领域:
药物化学
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分析化学
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PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
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2013
·
IF 4.612
Sheng Guo,Jin-ao Duan,Dawei Qian,Hanqing Wang,Yuping Tang,Yefei Qian,Dawei Wu,Shulan Su,Erxin Shang
In this study, a rapid and sensitive analytical method was developed for the determination of 20 nucleobases, nucleosides and nucleotides in Ziziphus plants at trace levels by using hydrophilic interaction ultra-high performance liquid chromatography coupled with triple-quadrupole tandem mass spectrometry (HILIC–UHPLC-TQ-MS/MS) in multiple-reaction monitoring (MRM) mode. Under the optimized chromatographic conditions, good separation for 20 target compounds were obtained on a UHPLC Amide column with sub-2 μm particles within 10 min. The overall LODs and LOQs were between 0.11–3.12 ng mL −1 and 0.29–12.48 ng mL −1 for the 20 analytes, respectively. It is the first report about simultaneous analysis of nucleobases, nucleosides and nucleotides in medicinal plants using HILIC–UHPLC-TQ-MS/MS method, which affords good linearity, precision, repeatability and accuracy. The developed method was successfully applied to Ziziphus plant ( Z. jujuba , Z. jujuba var. spinosa and Z. mauritiana ) samples. The analysis showed that the fruits and leaves of Ziziphus plants are rich in nucleosides and nucleobases as well as nucleotides, and could be selected as the healthy food resources. Our results in present study suggest that HILIC–UHPLC-TQ-MS/MS method could be employed as a useful tool for quality assessment of the samples from the Ziziphus plants as well as other medicinal plants or food samples using nucleotides, nucleosides and nucleobases as markers.
研究领域:
分析化学
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植物化学
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药用植物学
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PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2024
·
IF 3.8
Liang Lai,Mengyao Zhang,Tong Li,Jiahuan Qu,Dongsheng Xu,Pei Yu,Zhengjin Jiang
In this study, a novel piperidinium-sulfonate based zwitterionic hydrophilic monolith was prepared through thermally initiated co -polymerization of a piperidinium-sulfonate monomer 3-(4-((methacryloyloxy)methyl)-1-methylpiperidin-1-ium-1-yl)propane-1-sulfonate (MAMMPS), and a hydrophilic crosslinker N,N′ -methylenebisacrylamide (MBA) using n -propanol and H 2 O as porogenic system. Satisfactory mechanical and chemical stabilities, good repeatability and high column efficiency (120,000 N/m ) were obtained on the optimal monolith. The resulting poly(MAMMPS- co -MBA) monolith showed a typical HILIC retention behavior over an ACN content range between 5 and 95 %. Furthermore, this column exhibited good separation performance for various polar compounds. Compared to quaternary ammonium-sulfonate based zwitterionic hydrophilic monolith, i.e. poly(N,N-dimethyl-N-methacryloxyethyl-N-(3-sulfopropyl)ammonium betaine-co-MBA), the poly(MAMMPS- co -MBA) monolith displayed stronger retention and better selectivity for the tested phenolic and amine compounds at different pH conditions. Finally, this column was applied for the separation of six sulfonamide antibiotics, and the analytical characteristics of the method were evaluated in terms of precision, repeatability, limits of detection (LOD) and quantitation (LOQ). Overall, this study not only developed a novel HILIC monolithic column, but also proved the potential of piperidinium-sulfonate based zwitterionic chemistry as stationary phase, which further increased the structure diversity of zwitterionic HILIC stationary phases.
研究领域:
分析化学
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材料科学
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色谱学
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PubMed
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2016
·Vol. 408
·期 10
·2527-2542
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IF 3.125
Chen Jiahui,Hou Waner,Han Bo,Liu Guanghui,Gong Jin,Li Yemeng,Zhong Danmin,Liao Qiongfeng,Xie Zhiyong
Amino acids, neurotransmitters, purines, and pyrimidines are bioactive molecules that play fundamental roles in maintaining various physiological functions. Their metabolism is closely related to the health, growth, development, reproduction, and homeostasis of organisms. Most recently, comprehensive measurements of these metabolites have shown their potential as innovative approaches in disease surveillance or drug intervention. However, simultaneous measurement of these metabolites presents great difficulties. Here, we report a novel quantitative method that uses hydrophilic interaction ultra-high-performance liquid chromatography–tandem mass spectrometry (HILIC-UPLC–MS/MS), which is highly selective, high throughput, and exhibits better chromatographic behavior than existing methods. The developed method enabled the rapid quantification of 37 metabolites, spanning amino acids, neurotransmitters, purines, and pyrimidines pathways, within 6.5 min. The compounds were separated on an ACQUITY UPLC® BEH Amide column. Serum and brain homogenate were extracted by protein precipitation. The intra- and interday precision of all of the analytes was less than 11.34 %, and the accuracy was between −11.74 and 11.51 % for all quality control (QC) levels. The extraction recoveries of serum ranged from 84.58 % to 116.43 % and those of brain samples from 80.80 % to 119.39 %, while the RSD was 14.61 % or less for all recoveries. This method was used to successfully characterize alterations in the rat brain and, in particular, their dynamics in serum. The following study was performed to simultaneously test global changes of these metabolites in a serotonin antagonist p -chlorophenylalanine (PCPA)-induced anxiety and insomnia rat model to understand the effect and mechanism of PCPA. Taken together, these results show that the method is able to simultaneously monitor a large panel of metabolites and that this protocol may represent a metabolomic method to diagnose toxicological and pathophysiological states.
Overview of experimental workflow
研究领域:
生物化学
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医学
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分析化学
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PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2013
·
IF 4.612
Guangxin Yuan,Yongbo Peng,Zhenghua Liu,Jieya Hong,Yao Xiao,Jialiang Guo,Norman W. Smith,Jacques Crommen,Zhengjin Jiang
In order to prepare zwitterionic HILIC monolithic columns with high polarity, the highly hydrophilic monomer N , N -dimethyl- N -acryloyloxyethyl- N -(3-sulfopropyl)ammonium betaine (SPDA) and crosslinker N , N ′-methylenebisacrylamide (MBA) were employed for developing a novel sulfoalkylbetaine type stationary phase. The polymerization parameters were systematically optimized in order to obtain a satisfactory performance for column permeability, mechanical stability, hydrophilicity, efficiency and selectivity. Compared to the previously reported poly( N , N -dimethyl- N -methacryloxyethyl- N -(3-sulfopropyl)ammonium betaine- co -ethylene dimethacrylate) (poly(SPE- co -EDMA)) monolith and the poly(SPDA- co -EDMA) monolith that we developed, a significantly enhanced hydrophilicity was obtained on the poly(SPDA- co -MBA) monolithic column, illustrated by the lowered critical composition of the mobile phase corresponding to the transition from the HILIC to the RP mode. Excellent permeability, reproducibility and stability were achieved on this optimized poly(SPDA- co -MBA) monolith. A column efficiency of 70,000 plates/m was obtained for the analysis of bases at a linear velocity of 1.95 mm/s. As expected, by studying the influence of mobile phase pH and salt concentration on their retention, a weak electrostatic repulsion interaction for negatively charged analytes was also observed at low organic solvent content on the poly(SPDA- co -MBA) monolithic column. The final optimized poly(SPDA- co -MBA) monolith exhibited good selectivity for a series of polar compounds, such as phenols, bases, benzoic acid derivatives, small peptides, urea and allantoin.
研究领域:
分析化学
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材料科学
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PubMed
高影响因子
Analytical Methods
·
2021
·Vol. 13
·期 38
·4515-4527
·
IF 2.896
Zheng Gao,Ruizhi Tang,Shujuan Ma,Shicong Jia,Shuai Zhang,Bolin Gong,Junjie Ou
Although macroporous adsorbent resins (MARs) have been commercialized and widely applied in industrial and life fields, it is still of necessity to develop simple approaches to functionalize MARs. One of the most widely used methods to realize excellent fouling resistance performance is surface modification of hydrophilic polymers on substrates to fabricate an anti-biofouling coating. Herein, three kinds of hydrophilic poly(glycidyl methacrylate-co-ethylene glycol dimethacrylate) MAR were designed and facilely prepared by coating a layer of porous organic polymers (POPs) via either an epoxy–amine ring-opening polymerization or amine–aldehyde condensation reaction using isophthalaldehyde (IPA), 1,4,7,10-tetraazacyclododecane (cyclen), melamine and 1,3,5-triglycidyl isocyanurate (TGIC) as precursors. By taking advantage of their merits, such as large surface area, excellent hydrophilicity and unbiased affinity toward all types of glycopeptide, three functionalized hydrophilic MARs were successfully applied to capture glycopeptides from complex samples as hydrophilic interaction liquid chromatography (HILIC) sorbents. A total of 694 N-glycopeptides and 372 N-glycosylation sites were identified from 2 μL of human serum digest with poly(TC)@MAR, which were not only more than those of poly(MT)@MAR (286 N-glycosylation sites and 547 N-glycopeptides) and poly(IM)@MAR (669 N-glycopeptides and 355 N-glycosylation sites), but also more than those of other reported HILIC materials. This work provided a new and simple way to synthesize enrichment materials for liquid chromatography-mass spectrometry/mass spectrometry (LC-MS/MS) analysis of glycoproteomes.
研究领域:
生物化学
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分析化学
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蛋白质组学
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PubMed
高影响因子
Analytical Methods
·
2024
·Vol. 16
·期 5
·695-703
·
IF 2.7
Jiayi Wang,Xiaoya Zhang,Yinghua Yan,Rongrong Xuan
The comprehensive investigation of protein phosphorylation and glycosylation aids in the discovery of novel biomarkers as well as the understanding of the pathophysiology of illness. In this work, a nitrogen/titanium-rich porous organic polymer was developed by copolymerizing carbohydrazide (CH) and 2,3-dihydroxyterephthalaldehyde (2,3-Dha) and modifying with Ti4+ (CH–Dha–Ti4+). The adequate nitrogen contributes to the enrichment of glycopeptides via HILIC, while titanium benefits from capturing phosphopeptides through IMAC. The proposed method exhibits excellent selectivity (1 : 1000, both for glycopeptides and phosphopeptides), LOD (for glycopeptides: 0.05 fmol μL−1, for phosphopeptides: 0.2 fmol), loading capacity (for glycopeptides: 100 mg g−1, for phosphopeptides: 125 mg g−1) and size-exclusion effect (1 : 10 000, both for glycopeptides and phosphopeptides). Furthermore, CH–Dha–Ti4+ was applied to capture glycopeptides and phosphopeptides from human serum; 205 glycopeptides and 45 phosphopeptides were detected in the serum of normal controls; and 294 glycopeptides and 63 phosphopeptides were found in the serum of uremia patients after being analyzed by nano LC-MS/MS. The discovered glycopeptides and phosphopeptides were involved in several molecular biological processes and activities, according to a gene ontology study.
研究领域:
蛋白质组学
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生物化学
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分析化学
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PubMed
高影响因子
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