MICROCHIMICA ACTA
·
2018
·Vol. 185
·期 9
·1-10
·
IF 5.705
Zhou Xiu-Jie,Zhang Li-Shun,Song Wen-Fang,Huang Yan-Ping,Liu Zhao-Sheng
An inorganic-organic hybrid monolith incorporated with stellated mesoporous silica nanoparticles (SMSNs) was prepared. Using binary solvents, deep eutectic solvents and room temperature ionic liquids, an SMSN-incorporated poly(butyl methacrylate- co -ethylene glycol dimethacrylate) monolith demonstrated uniform structure with good column permeability. A systematic investigation of preparation parameter was performed, including SMSN content, crosslinking monomer content, and the component of binary solvent. The optimized monoliths were characterized by field emission scanning electron microscopy, transmission electron microscopy, area scanning energy dispersive spectrometry, and nitrogen adsorption. Column performance was tested by separating four groups of analytes (alkylbenzenes, anilines, naphthalenes and phenols) by capillary electrochromatography (CEC). Baseline separation of all analytes was obtained with column efficiencies of up to 266,000 plates m −1 . The performance of the resulting monolith was further investigated in detail by separating mixtures of polycyclic aromatic hydrocarbons (PAHs), nonsteroidal antiinflammatory drugs (NSAIDs), and hydroxybenzoic acid isomers. Compared with the corresponding SMSN-free monolith, the CEC performance was improved by about six times. Successful extraction of PAHs and quinolones (QNs) were also performed using this capillary. Improved extraction efficiency (20.2%) for complex samples, lake water, was also found when the material was applied to solid phase microextraction of fluoranthene.
A poly(butyl methacrylate-co-ethylene glycol dimethacrylate) monolith incorporated with stellated mesoporous silica nanoparticles was prepared. It demonstrated column efficiency up to 266,000 plates m −1 in capillary electrochromatography and ability as solid phase microextraction for organic small molecules with good column permeability.
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ACS Applied Materials & Interfaces
·
2023
·
IF 9.5
Wen-Chao Deng,Hai-Long Qian,Cheng Yang,Shu-Ting Xu,Xiu-Ping Yan
Covalent organic frameworks (COFs) are promising as stationary phases for gas chromatography (GC). The successful anchoring of COFs to the inner walls of the capillary with good uniformity is an important prerequisite to ensure the excellent separation performance of columns. However, current methods for the fabrication of COF-based capillary columns cannot always meet this requirement when faced with different COFs, which hampers the further development of COF-based GC stationary phases. Here, we show a general two-step method for the fabrication of COF-bound capillary column. The first step enables the formation of uniform amorphous polymer layer on the inner walls of capillary, while the second step allows the facile transformation of the amorphous polymer layer into a highly crystalline COF layer. COF-bound capillary columns with different framework structures were fabricated successfully by the developed two-step method. Impressively, the COF layers bound on the inner walls of these capillary columns showed good uniformity and high crystallinity. More importantly, as an example, the fabricated Tab-DHTA-bound capillary column showed good resolution (R > 1.5) and high column efficiency (700–39,663 plates m–1) for the tested isomers of ethylbenzene, xylene, dichlorobenzene, chlorotoluene, pinene, 1,3-dichloropropene, and propylbenzene with good precision (RSD, run-to-run, n = 5) (retention time, 0.2–0.6%; peak area, 0.5–1.1%; and peak height, 0.5–1.4%). In general, the fabricated Tab-DHTA-bound capillary column exhibited better performance for the separation isomers than commercial columns DB-5 and HP-FFAP. These results indicate that the two-step method is an efficient way to fabricate the COF-bound capillary column with excellent separation performance.
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JOURNAL OF CHROMATOGRAPHY A
·
2023
·
IF 4.1
Zhentao Li,Zhengzheng Liao,Xiaoru Ding,Jinfang Hu,Zilin Chen
Herein, a spherical covalent organic framework COF TAPB-DMTP was facilely synthesized from 2,5-dimethoxyterephthalaldehyde (DMTP) and 1,3,5-tri-(4-aminophenyl)benzene (TAPB) as monomers. COF TAPB-DMTP with regular mesoporous and excellent mass transfer ability was first introduced into the capillary and immobilized on the inner wall of the capillary through a simple in situ growth method. Through various characterization results, COF TAPB-DMTP was successfully prepared and modified onto the capillary inner wall. The separation performance and potential of COF TAPB-DMTP modified capillary column was explored. The new developed COF modified column achieved a highly efficiency and selective separation between analytes with different properties, including halogeno benzenes, alkylbenzenes, phenols and sulfonamides. Satisfactory stability and reproducibility were observed on COF TAPB-DMTP modified columns. The intraday, interday and three batch columns relative standard deviations were all less than 1.85 % for the retention time. The separation performance of prepared column has no significant change after 90 continuous runs. Additionally, the COF TAPB-DMTP modified capillary column was successfully used for separation and detection of triazole antifungal drugs in human plasma, and the recoveries of three antifungal drugs (fluconazole, isavuconazole and posaconazole) in spiked samples were in the range of 98.6–100.8 %, 92.4–102.1 % and 99.9–107.5 %, respectively. This self-made column showed excellent application potential in chromatography separation science.
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JOURNAL OF CHROMATOGRAPHY A
·
2023
·
IF 4.1
Yuanyuan Fu,Zhentao Li,Changjun Hu,Qiaoyan Li,Zilin Chen
A new kind of covalent organic framework (COF) was first utilized as an stationary phase for open-tubular electrochromatography (OT-CEC) by in situ synthesis immobilized method at room temperature. On the basis of our previous work, 4,4′,4″-(1,3,5-Triazine-2,4,6-triyl)trianiline (TZ) and 2,5-bis(2-propyn-1-yloxy)-1,4-benzenedicarboxaldehyde (BPTA) were employed as building blocks for the synthesis of COF TZ-BPTA. The coated capillary and COF TZ-BPTA were characterized by scanning electron microscopy (SEM). Then, Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), and X-ray diffraction (XRD) were also applied to characterize COF TZ-BPTA and the modified column. In SEM, it can be seen that COF TZ-BPTA was the spherical shape and the modified capillary was covered with globular particles equably. The COF TZ-BPTA coated column exhibited good separation resolution and efficiency towards two antiepileptic drugs and other kinds of small organic molecules involving alkylbenzene, sulfonamides, polycyclic aromatic hydrocarbon (PAH), parabens, amino acids and herbicides. The maximum column efficiency was over 2.8 × 10 5 plates·m −1 . In addition, the precisions (RSDs) of the retention times for the alkylbenzenes of intra-day runs (n = 3), inter-day runs (n = 3) and column-to-column runs (n = 3) were all less than 1.70% and separation performance was without obvious change within 100 times run. In addition, the real sample was tested on COF TZ-BPTA coated column. Hence, COF TZ-BPTA showed great potential in the separation domain.
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TALANTA
·
2023
·
IF 6.1
Haoyu Long,Yanhao Jiang,Yanjuan Liu,Yuefei Zhang,Wei Chen,Sheng Tang
In this work, 2,4,6-tris(4-aminophenyl)-1,3,5-triazine (TAPT) and 1,3,5-tris(4-formylphenyl)benzene (TFPB) were used as monomers to construct a triazine-containing imine-linked covalent organic framework (COF), which was then bonded onto the surface of aldehydized silica (SiO 2 –CHO), and finally a COF@silica composite material (TAPT-TFPB COF@SiO 2 ) was successfully prepared. The chromatographic separation performance of SiO 2 –CHO, TAPT-TFPB COF@SiO 2 and TAPT-TFPB COF@SiO 2 /SiO 2 –CHO (80/20, mass ratio) was evaluated and compared. It was found that separation efficiency was obviously enhanced by adding an appropriate amount of SiO 2 –CHO into TAPT-TFPB COF@SiO 2 . The obtained TAPT-TFPB COF@SiO 2 /SiO 2 –CHO showed more favorable separation ability than SiO 2 –CHO and TAPT-TFPB COF@SiO 2 . Various aromatic compounds including alkylbenzenes , polycyclic aromatic hydrocarbons , environmental endocrine disruptors , foodborne stimulants and phenyl ketones were effectively separated on the TAPT-TFPB COF@SiO 2 /SiO 2 –CHO column in reversed phase chromatography mode. The silica microspheres surface-modified with triazine-containing imine-linked COFs proved to be a new type of promising chromatographic packing materials.
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ACS Applied Materials & Interfaces
·
2023
·
IF 9.5
Tian-Tian Ma,Cheng Yang,Hai-Long Qian,Piming Ma,Tianxi Liu,Xiu-Ping Yan
Development of novel functional materials for effective isomer separation is of great significance in environmental science, chemical industry, and life science due to the different functions of isomers. However, the similar physicochemical properties of isomers make their separation greatly challenging. Here, we report the fabrication of trifluoromethyl-functionalized 2D covalent organic framework (COF) TpTFMB with 2,2′-bis(trifluoromethyl)benzidine (TFMB) and 1,3,5-triformylphloroglucinol (Tp) for the separation of isomers. TpTFMB was in situ-grown on the inner surface of a capillary for the high-resolution separation of isomers. The introduction of hydroxyl and trifluoromethyl functional groups with uniform distribution in 2D COFs is a powerful tactic to endow TpTFMB with various functions such as hydrogen bonding, dipole interaction, and steric effect. The prepared TpTFMB capillary column enabled the baseline separation of positional isomers such as ethylbenzene and xylene, chlorotoluene, carbon chain isomers such as butylbenzene and ethyl butanoate, and cis–trans isomers 1,3-dichloropropene. The hydrogen-bonding, dipole, and π–π interactions as well as the structure of COF significantly contribute to the isomer separation. This work provides a new strategy for designing functional 2D COFs for the efficient separation of isomers.
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JOURNAL OF CHROMATOGRAPHY A
·
2023
·
IF 4.1
Zhentao Li,Zhengzheng Liao,Jinfang Hu,Zilin Chen
Design of the smart stationary phases, which can improve the separation efficiency is an essential work in the capillary electrochromatography (CEC). Owing to good excellent properties, covalent organic frameworks (COFs) have showed promising potential in the area of separation science . Here, a micro- and mesoporous COF TAPB-BTCA with adequate available interaction sites and outstanding mass transfer performance was first exploited as a stationary phase for high-efficiency in capillary electrochromatography. Through in situ growth approach, the COF TAPB-BTCA coated capillary column was facilely prepared at room temperature . The separation ability of the COF TAPB-BTCA coated capillary column was studied. The fabricated column showed high efficiency for the separation of six types of small molecular compounds, including alkylbenzenes , chlorobenzenes , phenols, parabens , vanillin and related phenolic compounds , and non-steroidal anti-inflammatory drugs (NSAIDs). The maximum theoretical plates reached up to 293,363 N/m for phloroglucinol , showing significantly improved column efficiency in comparison to previous reported COFs-based columns. In addition, the mass loadability for methylbenzene was achieved to 1.44 mg/mL. Also, excellent reproducibility and stability were obtained on the COF TAPB-BTCA coated columns. The relative standard deviations of intra-day ( n = 3), inter-day ( n = 3) and three batch tubes were all less than 2%, and no obvious change was presented in separation performance after the column was used 120 runs. This COF TAPB-BTCA-based stationary phase would be a promising candidate for high-efficiency chromatographic separation.
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MICROCHIMICA ACTA
·
2019
·Vol. 186
·期 2
·1-8
·
IF 5.479
Li Zhentao,Mao Zhenkun,Chen Zilin
This work reports on the in-situ growth of a metal organic framework (MOF) composed of zinc(II), adeninate and biphenyldicarboxylate on the inner wall of a capillary, and the use of this MOF as a stationary phases in open-tubular capillary electrochromatography. The inner wall of a fused-silica capillary was first modified with 3-aminopropyltriethoxysilane to create surface amino sites, and then the MOF was synthesized by in-situ growth. The modified capillary was characterized by scanning electron microscopy, Fourier transform infrared spectroscopy and X-ray diffraction. The results proved the successful growth of the MOF. The resultant open-tubular column showed good separation selectivity towards neutral compounds, acidic and basic compounds including nonsteroidal anti-inflammatory drugs, sulfa drugs and small biomolecules. In addition, the modified column is stable and repeatable. The precisions (expressed as RSDs) of the retention time for intra-day ( n = 5) and inter-day (n = 5) separations and between columns ( n = 3) are less than 0.5, 1.6 and 4.7%, respectively. Conceivably, this new kind of MOF represents a most useful novel stationary phase in electrochromatographic separations.
Schematic presentation of the open-tubular column modified with bio-MOF-1 by in situ hydrothermal reaction with adeninate, Zn(II) and biphenyldicarboxylate for capillary electrochromatographic separations.
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JOURNAL OF CHROMATOGRAPHY A
·
2019
·
IF 3.858
Yike Huang,Gaoyi Yi,Baian Ji,Die Gao,Yuntian Bai,Yao Liu,Lujun Wang,Zhining Xia,Qifeng Fu
Mussel-inspired polydopamine (PDA) based materials are attractive as stationary phase for open-tubular capillary electrochromatography (OT-CEC) due to their many fascinating properties. However, all of the existing strategies for fabricating PDA based OT-CEC columns are limited in aqueous solutions. Consequently, it is a challenge work to directly immobilize the hydrophobic functional materials onto the inner wall of PDA modified capillary. Herein, by using the organic amine-inducing co-deposition strategy, a novel preparative method was developed for in situ one-pot synthesis of PDA/octadecylamine (ODA) co-deposited coating inside capillary as OT-CEC stationary phase. The formation and morphology of the PDA/ODA co-deposited coating were characterized by field emission scanning electron microscopy , atomic force microscope, attenuated total reflectance Fourier transform infrared spectroscopy and contact angle measurements. The separation performance of the fabricated PDA/ODA modified columns was validated by the separation of alkylbenzenes and steroids, which could achieve baseline separation with high separation efficiency. Their separation was found to follow the reversed phase chromatographic retention mechanism. The co-deposited column showed good stability and long lifetime. The repeatability of the PDA/ODA co-deposited column was also evaluated, with the relative standard deviations for intra-day and inter-day runs less than 5% and column-to-column runs less than 6%.
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ELECTROPHORESIS
·
2019
·
IF 2.754
Yuan-Yuan Cui,Huan Yao,Cheng-Xiong Yang,Xiu-Ping Yan
Microporous organic networks (MONs) are a new class of porous materials synthesized via Sonogashira coupling reactions between organic building blocks. Here we report an in situ synthesis approach to fabricate MONs coated capillary column for high resolution GC separation of hydrocarbons. The McReynolds constant evaluation reveals the MONs coated capillary is a non-polar column. The MONs coated capillary column shows good resolution for GC separation of diverse important industrial hydrocarbons such as linear and branched alkanes, alkylbenzenes, pinene isomers, ethylbenzene and styrene, cyclohexane and benzene. The MONs coated capillary column gave a high column efficiency of 1542 plates per meter for hexane and good precision for replicate separations of the selected hydrocarbons with the RSDs of 0.2–0.3, 1.5–3.1, and 1.9–3.3% for retention time, peak height and peak area, respectively. The MONs coated capillary also offered better resolution than commercial Inert Cap-1 and Inert Cap-5 capillary columns for hexane and heptane isomers. These results reveal the potential of MONs as novel stationary phases in GC.
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TALANTA
·
2019
·
IF 4.916
Xiaohui Yang,Guangping Wan,Shujuan Ma,Hongjun Xia,Jun Wang,Jiawei Liu,Yanna Liu,Gang Chen,Quan Bai
Recently, superficially porous particles (SPPs) have been intensively studied and employed for highly efficient and fast separations. In this paper, the SiO 2 @SiO 2 SPPs were synthesized by an improved polymerization-induced colloid aggregation (PICA) method using urea-formaldehyde polymer as the template. The agglomeration of silica core during modification with ureidopropyltrimethoxysilane (UPS) can not only be avoided by reflux in neutral ethanol solution, but also the secondary nucleation of the colloidal silica sol can be inhibited via optimizing the reaction conditions including pH, temperature, colloidal silica sol concentration and the reaction time. The shell thickness and pore size of SPPs can be controlled successfully by adjusting the weight ratio of silica core/colloidal silica sol and the particle size of colloidal silica sol, respectively. The SPP-C18 columns packed using octadecyltrichlorosilane (ODS) modified SPPs with different pore sizes were employed to separate small solutes and proteins. The baseline separations of 6 kinds of alkyl benzenes and 5 kinds of aromatic alcohol homologues were achieved within 4 min by the SPP-C18 column with 8 nm pore size. Compared with the commercial BEH-C18 column, more than 50,000/m of the plate number of propylbenzene was obtained, and the former provided higher column efficiency to separate small solutes than the latter. Meanwhile, 6 kinds of proteins were also separated completely within 2 min using the SPP-C18 column with 40 nm pore size. In addition, the SPP-C18 capillary column was applied to separate and identify the BSA/HeLa/mouse liver digests with capillary LC-MSMS, respectively. The results indicate that more proteins and peptides can be identified using SPP-C18 capillary column compared with commercial silica-C18 capillary column. The result demonstrates that the prepared SPP-C18 column provides higher column efficiency and the SPPs synthesized with the improved PICA method shows a great potential application for the fast separation of small solutes and proteins.
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ELECTROPHORESIS
·
2017
·Vol. 39
·期 2
·363-369
·
IF 2.744
Deying Kong,Zilin Chen
Pillar[ n ]arenes have achieved much interest in material chemistry and supramolecular chemistry due to unusual pillar shape structure and high selectivity toward guest. However, pillar[ n ]arenes have not yet been applied in capillary electrochromatography. This work at first time reports that carboxylatopillar[5]arene is used as a stationary phase in open-tubular capillary electrochromatography. Carboxylatopillar[5]arene not only possess the advantages of pillar[ n ]arenes but also provide free carboxy groups for immobilizing on the inner wall of capillary column via covalent bonding. The characterization of SEM and FT-IR indicated that carboxylatopillar[5]arene was successfully grafted on the inner wall of capillary. The baseline separation of model analytes including neutral, basic, and acidic compounds, nonsteroidal anti-inflammatory drugs and dansyl-amino acids have been achieved thanks to the electron-rich cavity of carboxylatopillar[5]arene and hydrophobic interactions between the analytes and stationary phase. The intraday, interday, and column-to-column precisions (RSDs) of retention time and peak area for the neutral analytes were all less than 3.34 and 9.65%, respectively. This work indicates that pillar[ n ]arenes have great potential in capillary electrochromatography as novel stationary phase.
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