JOURNAL OF CHROMATOGRAPHY A
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2017
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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
MICROCHIMICA ACTA
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2020
·Vol. 187
·期 7
·1-10
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IF 6.232
Zhang Xue,Shen Yan-Feng,Li Xin-Xin,Yang Jin-Rong,Liu Zhao-Sheng,Huang Yan-Ping
An organic-inorganic hybrid monolithic column doped with gold nanorods (AuNRs) was prepared and evaluated for solid phase extraction (SPE) of polycyclic aromatic hydrocarbons (PAHs). Excellent dispersibility of AuNRs in binary green porogen system consisting of 1-hexyl-3-methylimidazolium tetrafluoroborate and deep eutectic solvents (DESs) was confirmed by energy dispersive spectrometry (EDS). The particle size of the resulting AuNRs (70–90 nm) was thoroughly examined by a transmission electron microscopy (TEM). The redox system including ammonium persulfate (APS) and tetramethylethylenediamine (TEMED) was used to initiate in situ polymerization at 4 °C to prepare the hybrid monolith. The mesoporous structure of the AuNR hybrid monoliths was confirmed by scanning electron microscopy (SEM) and nitrogen adsorption. With enrichment factors (EFs) of 150- to 292-fold, the developed method was successfully applied to the determination of 10 PAHs in wastewater samples. The recoveries at a spiked level were in the range 84.9 to 99.5% with limit of detections (LODs) and relative standard deviations (RSDs) ranging from 0.02 to 0.10 μg L −1 and 1.5 to 4.2%, respectively. The correlation coefficients ( R 2 ) for the calibration function obtained were better 0.9991 for the target compounds. Compared to the AuNR-free monolith, the extraction efficiency of the AuNR-incorporated monolith is more than two times higher. The results indicated that the doping of AuNRs is an effective approach to obtain the hybrid monolithic column with good separation ability for PAHs.
Graphical abstract
研究领域:
分析化学
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环境科学
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PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2019
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IF 2.983
Wei Gao,Xiao-lan Liu,Jia-yuan Li,Hong-zhen Lian,Li Mao
A porous zwitterionic monolithic column was prepared to rapidly and efficiently separate lysozyme from egg white. The monolith was synthesized in a stainless steel HPLC column (5 cm × 4.6 mm i.d.) by in-situ thermal initiated co-polymerization of N,N- dimethyl -N- methacryloxyethyl- N -(3-sulfopropyl) ammonium betaine (MSA) and ethylene dimethacrylate (EDMA). Due to the combination of quaternary ammonium and sulfonic groups on the monolithic matrix in one-pot process, the hydrophobic carbon chain and hydrophilic radical were obtained, which provided multiple driving forces for neutral, basic and acidic analytes, thus mix-mode chromatography mechanism contributed to the retention of different charged proteins. Properties such as composition, morphology and stability of the MSA-co-EDMA monolithic column were characterized by various analytical methods and the results showed that the monolith has large through-pores, good hydrophilicity and permeability. The effects of mobile phase pH and ionic strength on proteins were investigated, drawing the conclusion that the main adsorption and elution mechanism of lysozyme on MSA-co-EDMA monolith was electrostatic interaction, while those of other proteins included hydrophobic, hydrophilic and electrostatic interactions. Therefore, efficient separation of lysozyme and other proteins could be successfully achieved by switching the pH of mobile phase. Lysozyme can be adsorbed using 20 mmol/L phosphate buffer (pH 7.0) and eluted with 20 mmol/L phosphate buffer (pH 2.0). To prove the practicality of the monolithic column, it was also applied in the separation of lysozyme in egg white, which means the work has the potential for further development in proteome analysis of real biological samples.
研究领域:
生物化学
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蛋白质组学
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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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2018
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IF 3.716
Manman Han,Wan Li,Rui Chen,Yangyang Han,Xiuhua Liu,Tingting Wang,Huaizhong Guo,Xiaoqiang Qiao
In this study, a novel amino acid and ionic liquid dual organically functionalized reagents modified polyhedral oligomeric silsesquioxane methacryl substituted (POSS-MA) based hybrid monolithic column (POSS-VBI-Cys) was designed and reported. With amino acid L-cysteine and ionic liquid 1-vinyl-3-butylimidazolium bromide as dual monomers, POSS-MA as the crosslinker, the new POSS-VBI-Cys hybrid monolithic column could be facilely fabricated via the “one-pot” free radical copolymerization and thiol-ene click reaction. Because of the introduction of polar amino acid L-cysteine, the new POSS-VBI-Cys column exhibited attenuated hydrophobicity in reversed-phase liquid chromatography separation. Polar amides, nucleosides and nucleic acid bases displayed strong retention on the POSS-VBI-Cys column and could be successfully separated. Furthermore, the new POSS-VBI-Cys column displayed good separation selectivity for model glycoproteins and non-glycoproteins mixture and it was also successfully used for the purification and separation of TARG1 protein from its originally expressed sample. In the future research, we will further exploit its performances for separation of intact proteins and in-depth proteome applications.
研究领域:
分析化学
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生物化学
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PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
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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
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2017
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IF 2.603
Doudou Zhang,Yu Zhao,Dandan Lan,Xiaomin Pang,Ligai Bai,Haiyan Liu,Hongyuan Yan
In this work a polymer monolithic column was fabricated within the confines of a stainless steel column (50 × 4.6 mm i.d.) via radical polymerization by using iron porphyrin and butyl methacrylate as co-monomers, ethylene glycol dimethacrylate as crosslinking agent, ethylene glycol, isopropyl alcohol and N, N-dimethylformamide as tri-porogens, benzoyl peroxide and N , N -dimethylaniline as initiators. The resulting monolithic column was characterized by elemental analysis , scanning electron microscopy, nitrogen adsorption BET surface area, and mercury intrusion porosimetry, respectively. Results showed that the homemade monolith occupied relatively uniform pore structure , low back pressure, and enhanced selectivity for proteins in complex bio-samples. The present work described a simple and efficient method for “fractionation separation” of human plasma proteins , and it is a promising separation method for complex bio-samples in proteomic research.
研究领域:
蛋白质组学
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生物化学
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PubMed
高影响因子
Food Analytical Methods
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2018
·Vol. 12
·期 3
·697-704
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IF 2.245
Cui Beijiao,Liu Haiyan,Yu Huan,Pang Xiaoya,Yan Hongyuan,Bai Ligai
In this paper, a hybrid monolithic column with modified nanodiamond and 1-dodecene as co-monomers was prepared and applied to the online enrichment and purification of β-sitosterol in edible oil. The obtained monolithic column was characterized by scanning electron microscopy (SEM) and nitrogen adsorption–desorption isotherm measurement, which indicated that the monolith possessed characteristics of porous structure and high permeability. Under the optimum conditions for extraction and determination, the linear regression coefficient for β-sitosterol was 0.998; the limit of detection (LOD) and the limit of quantitation (LOQ) were 3.0 μg mL −1 and 10.0 μg mL −1 , respectively; the relative standard deviation (RSD) of intra-day and inter-day assays for four edible oils were 2.33–6.58% and 3.24–6.94%, respectively. The recovery was in the range of 89.6–105.5%. The results showed that the hybrid monolithic column with high selectivity and good permeability were successfully used as online solid-phase extraction (SPE) column for determination of β-sitosterol in edible oil.
研究领域:
分析化学
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食品科学
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DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
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2015
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IF 4.169
Yuan Xiao,Jialiang Guo,Danni Ran,Qianqian Duan,Jacques Crommen,Zhengjin Jiang
A facile and efficient “one-pot” copolymerization strategy was used for the preparation of sulfonamide drug (SA) functionalized monolithic columns. Two novel SA-immobilized methacrylate monolithic columns, i.e. poly(GMA-SMX- co -EDMA) and poly(GMA-SAA- co -EDMA) were prepared by one-pot in situ copolymerization of the drug ligand (sulfamethoxazole (SMX) or sulfanilamide (SAA)), the monomer (glycidyl methacrylate, GMA) and the cross-linker (ethylene dimethacrylate, EDMA) within 100 μm i.d. capillaries under optimized polymerization conditions. The physicochemical properties and column performance of the fabricated monolithic columns were characterized by elemental analysis, scanning electron microscopy and micro-HPLC. Satisfactory column permeability, efficiency and separation performance were obtained on the optimized poly(GMA-SMX- co -EDMA) monolithic column for small molecules, such as a standard test mixture and eight aromatic ketones. Notably, it was found that the poly(GMA-SMX- co -EDMA) monolith showed a selective affinity to trypsin, while the poly(GMA-SAA- co -EDMA) monolith containing sulfanilamide did not exhibit such affinity at all. This research not only provides a novel monolith for the selective isolation and purification of trypsin, but it also offers the possibility to easily prepare novel drug functionalized methacrylate monoliths through a one-pot copolymerization strategy.
研究领域:
分析化学
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生物化学
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PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
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2016
·
IF 3.926
Zhenkun Mao,Zilin Chen
A novel monolithic column with ionic liquid and styrene-modified bifunctional group was prepared for capillary electrochromatography (CEC) by in situ copolymerization in a ternary porogenic solvent. Ionic liquid (1-allyl-methylimidazolium chloride, AlMeIm + Cl − ) and styrene served as the bifunctional monomer, while ethylene dimethacrylate (EDMA) was used as the cross-linker. The monomer of AlMeIm + Cl − was introduced as anion-exchange group, while styrene as hydrophobic and aromatic group; the similar conjugated structure in AlMeIm + Cl − and styrene was beneficial for offeing obvious synergistic effect. The bifunctional stationary phase possessed powerful selectivity for the separation of neutral compounds, acidic analytes and phenols. The highest column efficiency was 2.70 × 10 5 plates m −1 (theoretical plates, N) for toluene. A relatively strong electroosmotic flow (EOF) was obtained in a wide range of pH values from 2.0 to 12.0, which could successfully achieve the rapid separation of the analytes within 10 min. The proposed monolithic column was characterized by scanning electron microscopy (SEM) and Fourier transform infrared (FT-IR). The results indicated that the resultant monolithic column had good permeability and excellent mechanical stability. Good reproducibility was obtained with relative standard deviations (RSDs) of the retention time in the range of 0.24–0.47% and 0.81–2.17% for run-to-run (n = 5) and day-to-day (n = 5), while 1.09–2.70% and 0.98–1.70% for column-to-column (n = 3) and batch-to-batch (n = 3), respectively. The combination of AlMeIm + Cl − and styrene was a promising option in the fabrication of the organic polymer monolithic column.
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 B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2019
·
IF 2.813
Mingxue Li,Ligai Bai,Shan Peng,Fanrong Sun,Laisen Wang,Haiyan Liu,Hongyuan Yan
A polymer-based chromatographic monolithic column was prepared via in-situ radical polymerization using tetrahydrofurfuryl methacrylate as the monomer . The homemade column was used for the separation and quantitative analysis of alkaloids, including piperine from Piper longum (fruit of Piper longum Linn .) and pepper (fruit of Piper nigrum L. ), hydroxy-α-sanshool, and hydroxy-γ-sanshool from zanthoxylum (fruit of Zanthoxylum bungeanum Maxim ), as well as caffeine from Wuyi rock tea. The chromatographic fractions were identified by mass spectrometry. Single factor test and orthogonal test were both carried out to optimize the extraction conditions. The method validation indicated that the accuracy represented by spiked recovery ranged in 98.89%–102.06%, the correlation coefficients in 0.99986–0.99999. These results show that the prepared monolithic column can be successfully used to quantitatively analyse alkaloids from the real medicinal and edible plant foods with reversed-phase mechanism, which can avoid the long analytical time using traditional packed C18 column. The present method is a simple, and inexpensive method for quantitatively analysing alkaloids from medicinal and edible plant foods, exhibiting good specificity and durability.
研究领域:
药学
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分析化学
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PubMed
高影响因子
TALANTA
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2019
·
IF 4.916
Chen Ma,Shujuan Ma,Yao Chen,Yan Wang,Junjie Ou,Jing Zhang,Mingliang Ye
A fast and robust approach was developed to fabricate and modify hybrid monolithic columns via two-step photo-initiated reactions. At first, acrylopropyl polyoctahedral silsesquioxane (acryl-POSS) and 3-(triallyl silyl) propyl acrylate (TAPA) were chosen as precursors to synthesize poly (POSS- co -TAPA) monolithic column (monolith I) via photo-initiated free-radical polymerization within 10 min, which left lots of allyl groups on the surface of monolith. Secondly, two thiol-containing compounds, penicillamine and 1-octadecanethiol (ODT), were introduced to modify the prepared poly (POSS- co -TAPA) column via photo-initiated thiol-ene click reaction within 20 min. Finally, three resulting monolithic columns were applied to separate phenolic, anilines and antibiotics mixtures. These mixtures were baseline-separated on the monolith modified with penicillamine (monolith II), exhibiting better selectivity than both pristine monolith I and that modified with ODT (monolith III). Additionally, these columns were further used for separation of tryptic digest of HeLa cells by cLC-MS/MS. The 5071 unique peptides mapped to 2442 proteins were identified from HeLa cells digest on monolith II, which were superior over those on monolith III, but slightly lower than those on monolith I. These results demonstrated that these POSS-containing columns exhibited great separation ability for complex samples.
研究领域:
分析化学
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生物化学
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PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
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2014
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IF 4.258
Qiqin Wang,Jun Feng,Hai Han,Peijie Zhu,Huihui Wu,Maria Luisa Marina,Jacques Crommen,Zhengjin Jiang
In order to obtain satisfactory column permeability, efficiency and selectivity for micro-HPLC, a capillary monolithic column containing O -9-[2-(methacryloyloxy)-ethylcarbamoyl]-10,11-dihydroquinidine (MQD) as chiral selector was re-optimized. The monolithic column was used to successfully enantioresolve a wide range of N-derivatized amino acids including alanine, leucine, methionine, threonine, phenylalanine, valine, serine, isoleucine, tryptophan, and cysteine. The influence of mobile phase parameters, such as the organic solvent type and concentration, the apparent pH, and buffer concentration, on retention and enantioseparation of N-derivatized amino acids has been investigated. 3,5-dinitrobenzoyl-amino acids and 3,5-dichlorobenzoyl-amino acids were resolved into enantiomers with exceptionally high selectivity and resolution. The chemoselectivity of the monolithic column for a multicomponent mixture of N-derivatized amino acids was also investigated. A mixture of three pairs of 3,5-dichlorobenzoyl-amino acids could be fully resolved in 22.5 min.
研究领域:
分析化学
·
色谱技术
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DOI
高影响因子
危险品化学品经营许可证（带存储）