TALANTA
·
2021
·
IF 6.057
Wenqi Sun,Yikun Liu,Wei Zhou,Zhentao Li,Zilin Chen
Column technology is an important part in capillary electrochromatographic science. Developing novel stationary phase with high separation efficiency and high loading capacity is an essential work. In this work, a novel spherical vinyl-functionalized covalent-organic framework (COF–V) was synthesized at room temperature and firstly employed as stationary phase for CEC-MS analysis. The COF–V based CEC column was characterized by scanning electron microscopy, X-ray diffraction and Fourier transform infrared spectroscopy. The results proved the successful modification of COF–V. The COF–V based column possesses the advantages like strong electroosmotic flow , high separation efficiency and high loading capacity. The CEC column showed powerful separation selectivity to several kinds of compounds, and the highest column efficiency (theoretical plates, N) was over 1.4 × 10 5 plates·m −1 for methylbenzene . Besides, the COF–V modified column exhibited excellent repeatability and stability. The relative standard deviations (RSDs) of retention times for intra-day (n = 5), inter-day (n = 3) runs and column-to-column (n = 3) were all less than 2.1%. Hence, the COF–V modified column was successfully applied in CEC-MS for determination of antiepileptic drug , triazine herbicides and active ingredients in traditional Chinese medicine.
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高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2021
·
IF 4.759
Yuanyuan Fu,Zhentao Li,Qiaoyan Li,Changjun Hu,Yikun Liu,Wenqi Sun,Zilin Chen
Covalent organic frameworks (COFs), considered as a series of newly emerging porous organic materials, have been widely utilized in separation fields. Herein, a novel COF (TFPB-BD) was first employed as stationary phase for high-efficiency capillary electrochromatographic separation. Benzidine (BD) and 1,3,5-Tris-(4-formylphenyl)benzene (TFPB) were selected as organic linkers and then introduced into the aldehyde group modified capillary for the in situ growth of TFPB-BD onto the capillary inner wall at room temperature. The morphology and formation of TFPB coated capillary column were confirmed by a variety of tools including Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) and energy dispersive X-ray spectrometry (EDS). It's interesting that the TFPB globular crystals with nanoscale were uniformly and densely modified on the capillary inner surface. Hence, the prepared column exhibited prominent separation performance for the test analytes including alkylbenzenes, chlorobenzenes and phenolic compounds with high efficiency and high resolution. The maximum column efficiency can reach about 1.8 × 10 5 plates•m −1 . Additionally, the high resolutions of anilines, amino acids and parabens were also achieved on the TFPB modified capillary. The precisions (RSDs) of the retention times of alkylbenzenes of intra-day runs ( n = 3), inter-day runs ( n = 3) and parallel columns ( n = 3) were all less than 2.83%. This innovative COF-based stationary phase gives great promise for the chromatographic separation field.
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JOURNAL OF CHROMATOGRAPHY A
·
2021
·
IF 4.759
Changjun Hu,Zhenkun Mao,Zhentao Li,Qiaoyan Li,Zilin Chen
Hydrophilic column combined with mobile phase containing high content of water is a green method for the separation of polar compounds, but there are few related studies, and the separation efficiency and performance of existing columns still needs to be improved. In this work, a novel monolithic column for separation of hydrophilic compounds under both high water content and HILIC condition, was prepared by in-situ polymerization using 4-vinylbenzoic acid (VBA) and 1-(Acryloyloxy)-3-(methacryloyloxy)-2-propanol (AMAP) as functional monomers. The poly(VBA- co -AMAP) monolithic column showed good separation performance towards various polar compounds under different chromatographic conditions based on the π-interaction, hydrophobic and hydrogen bonding interactions provided by 4-vinylbenzoic acid functional monomer. The highest column efficiency for adenine was over 2.15 × 10 5 plates m −1 (theoretical plate, N). In addition, the monolith showed good stability and reproducibility, the relative standard deviations (RSDs) of retention times within days (n = 5), between days (n = 5), between columns (n = 3) and between batches (n = 3) were 0.47-1.13%, 1.20-2.68%, 0.59-1.78% and 1.54-3.60%, respectively. This novel type of monolith has great application potential in the separation of hydrophilic compounds.
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高影响因子
AICHE JOURNAL
·
2021
·Vol. 67
·期 6
·e17197
·
IF 3.993
Liyun Huang,Kui Wu,Qian He,Chao Xiong,Tao Gan,Xiaohui He,Hongbing Ji
Single atom catalysts (SACs), featured with atomically dispersed metal species, have been considered as one of the most promising catalytic materials because of the excellent performance in various high-value-added reactions. However, the large-scale and continuous-type production of such SACs is still challenging. Herein, a novel and facile microcapsule strategy for the quasi-continuous synthesis of iron SACs supported on S, N co-doped carbon (Fe/SNC) is developed, and the Fe species are presented as isolated active sites and stabilized as the FeN 3 S-like structure. The as-prepared Fe/SNC catalysts exhibit excellent catalytic properties for selective oxidation of arylalkanes, which followed pseudo-first-order kinetics with an E a = 41.5 kJ/mol. More importantly, the two Fe/SNC catalysts synthesized at different continuous times showed essentially identical catalyst structure and catalytic performance, demonstrating the superior reliability of our microcapsule strategy for the quasi-continuous production of SACs, which can be easily scaled up to industrial application.
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高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2020
·
IF 4.049
Xingyun Zhao,Hongyan Zhang,Xiaoyu Zhou,Li Wang,Lihong Wan,Ren'an Wu
Hydrothermally cross-linked polyvinylpyrrolidone (PVP) immobilized SiO 2 stationary phase (CPVP-Sil) was prepared via a green and facile one-pot method which was demonstrated for hydrophilic interaction liquid chromatography (HILIC) as well as reverse phase chromatography(RP). A water or organic solvent-insoluble permanent CPVP immobilizing on the silica particle surface can be formed simply by dipping silica particles into PVP solution and low temperature hydrothermal treatment. The cross-linked PVP network coating on SiO 2 endow it ring lactam functional groups which exhibited excellent separation ability of polar compounds by a typical HILIC retention mechanism at higher organic solvent contents (>55% ACN) and additionally polyvinyl groups for separation of alkylbenzenes in RP mode(<25% ACN). A high column efficiency of about 7 × 10 4 plates per meter was obtained for the test catechol compound. Remarkably, the CPVP-Sil packing materials showed good stability in acid (at pH 3.5) or basic (at pH 9.5) conditions, with 5400-fold column volumes and 3500-fold column volumes respectively.
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TALANTA
·
2020
·
IF 5.339
Xue Li,Yuan-Yuan Cui,Cheng-Xiong Yang
Microporous organic networks (MONs) have shown great promise in separation science recently. Exploring novel, simple and convenient strategy to fabricate MONs coated capillary columns for gas chromatography (GC) still remains challenging but desirable for the development of MONs in chromatographic separation. To extend the potential application of MONs in separation science and to further develop novel method for the fabrication of MONs-based capillary columns, here we demonstrate a novel covalent coupling strategy to fabricate uniform MONs bonded capillary columns for GC separation of position isomers and hydrocarbons. The bare capillary column was firstly modified with (3-bromopropyl)trimethoxysilane to provide bromine sites for coupling with alkynyl monomers . The amino- and hydroxyl-functionalized MONs (MON-NH 2 and MON-OH) were then directly grown onto the inner wall of the brominated capillary columns via the covalent coupling between bromine and alkynyl groups. The uniform MON-NH 2 and MON-OH bonded capillary columns were obtained and showed good resolution for GC separation of dichlorobenzene , chlorotoluene, bromotoluene, and propylbenzene position isomers and many other hydrocarbons including linear alkanes, alkylbenzenes , pinene isomers, cyclohexane and benzene, ketones and aldehydes. The MONs bonded capillary columns also owned good lifetime and precision for dichlorobenzene isomers with the relative standard deviations (RSDs) of 0.2–0.3%, 1.2–2.1%, and 1.7–2.5% for retention time, peak height and peak area, respectively. In addition, the fabricated MON-NH 2 and MON-OH bonded capillary columns offered better resolution than commercial InertCap-1, InertCap-5, InertCap-1701 and InertCap-WAX capillary columns for the separation of chlorotoluene and bromotoluene position isomers. These results revealed the feasibility of covalent coupling strategy to fabricate MONs-based stationary phases in GC, highlighting the potential of MONs in separation science.
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JOURNAL OF CHROMATOGRAPHY A
·
2020
·
IF 4.049
Zhentao Li,Zhenkun Mao,Changjun Hu,Qiaoyan Li,Zilin Chen
Fluorous affinity means remarkably specific interaction between highly organic fluorides. This work aims to explore the potential of fluoro-functionalized stationary phase for the separation of organic fluorides by means of fluorous-fluorous interaction. Here, by using the Michael addition strategy between 1H,1H,2H,2H-perfluorodecanethiol (PFDT) and polydopamine (PD), a novel fluoro-functionalized stationary phase was synthesized for open-tubular capillary electrochromatography (OT-CEC). The PFDT@PD was characterized by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR) and X-ray Photoelectron Spectrometer (XPS). The PFDT@PD@capillary exhibited outstanding separation performance towards neutral compounds (such as alkylbenzenes and chlorobenzenes) and organic fluorides (such as fluorobenzenes and perfluoroalkyl methacrylates etc.) with high resolution and high separation efficiency by hydrophobic interaction and fluorous-fluorous interaction. In addition, the column shows good stability and reproducibility. The relative standard deviations (RSDs) of the retention time for intra-day (n = 5) and inter-day (n = 3) runs and between columns (n = 3) are less than 0.39%, 1.22% and 3.87%, respectively. This novel type of fluoro-functionalized stationary phase represents a great application potential in organic fluorides separation field.
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JOURNAL OF CHROMATOGRAPHY A
·
2019
·
IF 3.858
Zhihua Song,Shenghong Li,Yafeng Guan,Shuo Wang,Yinghao Wang,Gangqiang Yang,Xiaochen Zhang,Jinhua Li,Wenhao Song,Chuanming Zhou,Lingxin Chen
In this work, multilayer zirconia-coated silica (ZrO 2 /SiO 2 -n) microspheres were successfully produced by a straightforward hydrothermal procedure with a low concentration of Zr 4+ (5 mM) under low potential of hydrogen (pH) conditions (pH = =2). The obtained ZrO 2 /SiO 2 -n materials exhibited favorable characteristics for high-performance liquid chromatography (HPLC) separation, including high surface area and pore volume, good pore structure, narrow particle size, and pore size distribution. In addition, the zirconia coverage in the mesopores was confirmed by soaking the material in 1 M NaOH solution, with the particles showing strong resistance to the basic solution. The obtained ZrO 2 /SiO 2 -n stationary phases were packed into a fused-silica capillary tubing for the separation of alkaloids in hydrophilic interaction chromatography (HILIC) mode, and a column efficiency of 47,800 plates/m was obtained for berberine on a ZrO 2 /SiO 2 -6 micro column. The ZrO 2 /SiO 2 -6 microspheres were further modified by dodecylphosphonic acid (C 12 P-2-ZrO 2 /SiO 2 -6); the C 12 P-2-ZrO 2 /SiO 2 -6 material showed great potential for application in reversed-phase liquid chromatography (RPLC) mode. The C 12 P-2-ZrO 2 /SiO 2 -6 micro column showed a column efficiency of 55,000 plates/m for naphthalene and 51,300 plates/m for benzene.
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Separation Science Plus
·
2019
·Vol. 2
·期 12
·432-439
·
IF 0
Yu-Yu He,Qing Pu,Jun-Hui Zhang,Sheng-Ming Xie,Xue-Xian Chen,Li-Ming Yuan
Mesoporous materials are promising functional materials due to their properties, such as a large surface area, tunable pore size, structure and morphology. Chiral mesoporous silica is an indispensable part of mesoporous materials. Considering that chirality is rare in inorganic mesoporous materials, there are very few reports on chiral inorganic mesoporous silica for chromatographic separations. In this work, we report the use of chiral inorganic mesoporous silica based on the template of myristyl chloride- l -valine sodium as the stationary phase for enantioselective separation in gas chromatography. Thirteen chiral compounds were resolved on a fabricated column using dynamic coating, including chiral alcohols, epoxides and amino acid derivatives. In addition, n -alkanes, n -alcohols and aromatic hydrocarbons have also been separated.
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CHIRALITY
·
2019
·Vol. 31
·期 12
·1053-1059
·
IF 1.927
Yu-Yu He,Jun-Hui Zhang,Qing Pu,Sheng-Ming Xie,Yan-Xia Li,Lan Luo,Xue-Xian Chen,Li-Ming Yuan
Chiral mesoporous silica (CMS) has attracted widespread attention because of some unique properties, such as high surface area, uniformly structured nanoscale cavities, and excellent chemical and thermal stability. In this work, we report the utilization of a CMS as the stationary phase for the separation of racemates in gas chromatography (GC). A CMS-coated capillary column was fabricated by a dynamic coating method. Eighteen racemates belonging to different classes of organic compounds were separated on this column, including chiral alcohols, aldehydes, ketones, organic acids, halohydrocarbons, alkenes, alcohol amines, epoxides, and amino acid derivatives. In addition, linear alkanes, alcohols, and aromatic hydrocarbons have also been resolved.
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MICROCHIMICA ACTA
·
2019
·Vol. 187
·期 1
·1-8
·
IF 5.479
Xi Ying,Du Yingxiang,Sun Xiaodong,Zhao Shiyuan,Feng Zijie,Chen Cheng,Ding Wen
A monolithic capillary column was prepared by single-step copolymerization of the ionic liquid 1-vinyl-3-octylimidazolium bromide (VOI) and styrene. The VOI and styrene monomers were introduced to provide multiple interaction sites and increase hydrophobicity and aromaticity of the monolithic column, respectively. The effect of porogen ratio, monomer ratio and reaction temperature on permeability was investigated. The resulting column was characterized by scanning electron microscopy, and the results suggest that the column possesses high porosity and good homogeneity. A relatively strong anodic electroosmotic flow was generated over a wide range of pH values (pH 2.0–10.0), and this facilitates the rapid separation of analytes within 12 min. Alkylbenzenes, polycyclic aromatic hydrocarbons (PAHs), proteins and amino acids were used to evaluate the performance of the monolithic column under capillary electrochromatography mode by UV detection. Mixed-mode retention mechanisms including hydrophobic interaction, π-stacking, ion-exclusion interaction were observed. The monolithic column exhibits high column efficiency (8.72 × 10 4 plates∙m −1 ) and satisfying separation capability (the resolution of four alkylbenzenes: 2.54, 2.86 and 4.62, four PAHs: 2.79, 4.83 and 4.77, three proteins: 4.35 and 2.86, two amino acids: 3.34).
Schematic representation of capillary electrochromatography (CEC) systems with ionic liquid and styrene based organic polymer monolithic column for separation of alkylbenzenes, polycyclic aromatic hydrocarbons, proteins and amino acids.
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Journal of Pharmaceutical Analysis
·
2022
·
IF 14.026
Yikun Liu,Ning He,Yingfang Lu,Weiqiang Li,Xin He,Zhentao Li,Zilin Chen
Here, a styrene-based polymer monolithic column poly(VBS- co -TAT- co -AHM) with reversed-phase/hydrophilic interaction liquid chromatography (RPLC/HILIC) bifunctional separation mode was successfully prepared for capillary electrochromatography by the in situ polymerization of sodium p-styrene sulfonate (VBS) with cross-linkers 3-(acryloyloxy)-2-hydroxypropyl methacrylate (AHM) and 1,3,5-triacryloylhexahydro-1,3,5-triazine (TAT). The preparation conditions of the monolith were optimized. The morphology and formation of the poly(VBS- co -TAT- co -AHM) monolith were confirmed by scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FT-IR). The separation performances of the monolith were evaluated systematically. It should be noted that the incorporation of VBS functional monomer can provide π−π interactions, hydrophilic interactions, and ion-exchange interactions. Hence, the prepared poly(VBS- co -TAT- co -AHM) monolith can achieve efficient separation of thiourea compounds, benzene series, phenol compounds, aniline compounds and sulfonamides in RPLC or HILIC separation mode. The largest theoretical plate number for N , N′ -dimethylthiourea reached 1.7 × 10 5 plates/m. In addition, the poly(VBS- co -TAT- co -AHM) monolithic column showed excellent reproducibility and stability. This novel monolithic column has great application value and potential in capillary electrochromatography (CEC).
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