JOURNAL OF SEPARATION SCIENCE
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2015
·Vol. 38
·期 11
·1813-1821
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IF 2.737
Qiaoxuan Zhang,Jialiang Guo,Yuan Xiao,Jacques Crommen,Zhengjin Jiang
To further evaluate the feasibility and applicability of the one-pot strategy in monolithic column preparation, two novel β-cyclodextrin-functionalized organic polymeric monoliths were prepared using two β-cyclodextrin derivatives, i.e. mono(6-amino-6-deoxy)-β-cyclodextrin and heptakis(6-amino-6-deoxy)-β-cyclodextrin. In this improved method, mono(6-amino-6-deoxy)-β-cyclodextrin or heptakis(6-amino-6-deoxy)-β-cyclodextrin reacted with glycidyl methacrylate to generate the corresponding functional monomers and were subsequently copolymerized with ethylene dimethacrylate. The polymerization conditions for both monoliths were carefully optimized to obtain satisfactory column performance with respect to column efficiency, reproducibility, permeability, and stability. The obtained poly(glycidyl methacrylate-mono(6-amino-6-deoxy)-β-cyclodextrin- co -ethylene dimethacrylate) and poly(glycidyl methacrylate-heptakis(6-amino-6-deoxy)-β-cyclodextrin- co -ethylene dimethacrylate) monoliths exhibited a uniform structure, good permeability, and mechanical stability as indicated by scanning electron microscopy and micro-high-performance liquid chromatography experimental results. Because of the probable existence of multi-glycidyl methacrylate linking spacers on the poly(glycidyl methacrylate-heptakis(6-amino-6-deoxy)-β-cyclodextrin- co -ethylene dimethacrylate) monolith, the effect of the ratio of glycidyl methacrylate/heptakis(6-amino-6-deoxy)-β-cyclodextrin was especially studied, and satisfactory reproducibility could still be achieved by strictly controlling the composition of the polymerization mixture. To investigate the effect of the degree of amino substitution of β-cyclodextrin on column performance, a detailed comparison of the two monoliths was also carried out using series of analytes including small peptides and chiral acids. It was found that the β-cyclodextrin-functionalized monolith with mono-glycidyl methacrylate linking spacers demonstrated better chiral separation performance than that with multi-glycidyl methacrylate linking spacers.
研究领域:
分析化学
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材料科学
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DOI
PubMed
高影响因子
ANALYTICA CHIMICA ACTA
·
2024
·
IF 5.7
Tong Chen,Ye Shu,Guangsan Song,Tao Liu,Jun Jiang,Bingxin Jiang,Xufang Zong,Zihan Zhao,Baixiu Zhao,Yichen Zeng
Background Hydrophilic Interaction Liquid Chromatography (HILIC) is an outstanding strategy for the challenging analysis of hydrophilic and polar components. Nevertheless, analysis under HILIC mode typically consumes 70%–95 % acetonitrile with the disadvantage of high analytical costs, being environmentally unfriendly and causing biohazards, which is not in line with the concept of green chromatography. Research has shown that Per Aqueous Liquid Chromatography (PALC) simultaneously emphasizes efficient analytical performance for hydrophilic analytes and green analytical concepts. The development of new PALC stationary phases with superior performance is necessary. Results In this paper, silanized silica was sequentially subjected to esterification reaction, polymerization reaction and covalent bonding through five steps to obtain SiO 2 -RHP-AuNPs material, which was prepared as a novel stationary phase for PALC. Comprehensive characterization of the materials by means of Fourier transform infrared spectroscopy, Transmission scanning electron microscope, Elemental analysis and Thermogravimetric analysis showed the successful bonding of the functionalized groups on the original silica. The polymeric stationary phase based on Radix hedysari polysaccharide and Au nanoparticles had higher density of hydroxyl and ester functionalized groups. The Au nanoparticles upgraded their mesoporous structure and thermal stability, providing exceptional chromatographic performance and selectivity for chromatographic analysis. The influence of mobile phase water content, salt concentration, pH and column temperature on the retention behavior was evaluated. The novel Column was found to exhibit a dual mechanism of hydrophobic interactions/ion exchange interactions in a mobile phase with high water content. Significance and novelty The separation efficiency and selectivity of SiO 2 -RHP-AuNPs columns for synthetic pigments and organic acids in PALC mode were superior to those of commercial HILIC and C 18 columns. In addition, a method for the determination of seven active ingredients in Fructus Ligustri Lucidi by SiO 2 -RHP-AuNPs column in PALC mode was developed. The method had good stability, reproducibility and accuracy, which was capable of realizing the quality evaluation of Chinese Materia Medicas.
研究领域:
分析化学
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中药学
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PubMed
高影响因子
ANALYTICA CHIMICA ACTA
·
2022
·
IF 6.911
Wen-Bo Xie,Hao Li,Lei Zeng,Li-Juan Jiang,Wen Li,Lu Xia,Fu-Hou Lei
A column prepared using a unique three-membered phenanthrene skeleton of rosin has complementary selectivity to a C18 column for some separation tasks. In this study, propylene pimaric acid (16-hydroxyethyl acrylate-34-n-butyl) ester (BRB) and propylene pimaric acid (16-hydroxyethyl acrylate-34-dodecyl) ester (BRLA) were used as functional ligands to prepare two novel stationary phases, namely BRB@SiO 2 and BRLA@SiO 2 , through a “thiol-ene” click chemistry reaction. The characterization results of Fourier transform infrared spectroscopy , thermogravimetric analysis , nitrogen adsorption-desorption measurements, and contact angle tests showed that the BRB@SiO 2 and BRLA@SiO 2 stationary phases were successfully prepared. In addition, the performance of the columns was evaluated using the Tanaka test and hydrophobic subtraction model, which showed that the stationary phases exhibited typical reversed-phase chromatography performance and good hydrophobicity , hydrophobic selectivity , and steric selectivity. The changes in the retention of Panax notoginseng saponins on a column under different chromatographic conditions (acetonitrile content, flow rate , and column temperature) were investigated. The separation effect of BRB@SiO 2 and BRLA@SiO 2 columns on P. notoginseng saponins was better than that of the C18 column and the BRLA@SiO 2 column could replace the C18 column for the detection of P. notoginseng saponins.
研究领域:
分析化学
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药学
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PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
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2021
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IF 4.759
Yang Zhao,Jing Wang,Yang Yang,Qing Fu,Yanxiong Ke
In this work, mesoporous silica microspheres with bimodal porous structures for size exclusion chromatography (SEC) supports were synthesized via a pseudomorphic transformation method by using 3.5 and 5 μm commercial silica particles as sources and cetyltrimethylammonium bromide (CTAB) as a template. The effects of the synthetic conditions on the pore size distribution were examined, including the temperature, reaction time and the molar ratio of SiO 2 :NaOH. Bimodal porous silicas (BPSs) with pore sizes of 3.01 and 12.80 nm were obtained with SiO 2 :NaOH:CTAB:H 2 O=1:0.1:0.1:20 at 80 °C for 24 h. The BPSs were bonded with diol groups to produce a stationary phase for SEC. The column performance was evaluated with three types of samples, namely, dextran (70 KDa-62 Da), polyethene glycol (PEG) (20 KDa-32 Da) and three biomolecules (36 KDa-1.36 KDa). The column that was packed with a 3.5 μm stationary phase showed excellent resolution for molecular weights of less than 1 KDa with high column efficiency. Carbohydrate samples (dextran (MW=1296), dextran (MW=972), sucrose (MW=342), glucose (MW=180) and glycerol (MW=92)) were separated. Heptaethylene glycol, hexaethylene glycol, pentaethylene glycol, tetraethylene glycol, triethylene glycol, and diethylene glycol were resolved in a PEG200 sample. In summary, this work shows the advantages of bimodal mesopores in SEC for small molecules less than 1 kDa. In the pseudomorphic synthesis, the pore size can be regulated by template micelles. Thus, the development SEC supports with high accuracy for a specified molecular weight range is expected since the pore size can be regulated by the surfactant template.
研究领域:
材料科学
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分析化学
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纳米技术
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高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2017
·Vol. 40
·期 23
·4521-4529
·
IF 2.557
Haixia Lyu,Heqing Zhao,Wenfei Qin,Zenghong Xie
A simple “one-pot” approach for the preparation of a new vinyl-functionalized organic–inorganic hybrid monolithic column is described. In this improved method, the hydrolyzed alkoxysilanes of tetramethoxysilane and triethoxyvinylsilane were used as precursors for the synthesis of a silica-based monolith, while 1-hexadecene and sodium ethylenesulfonate were used as vinyl functional monomers along with azobisisobutyronitrile as an initiator. The effects of reaction temperature, urea content, and composition of organic monomers on the column properties (e.g. morphology, mechanical stability, and chromatographic performance) were investigated. The monolithic column was used for the separation of neutral solutes by reversed-phase pressurized capillary. Furthermore, the monolith can separate various aromatic amines, which indicated its excellent cation-exchange capability and hydrophobic interactions. The baseline separation of the aromatic amines was obtained with a column efficiency of up to 78 000 plates/m.
研究领域:
分析化学
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色谱学
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电化学
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材料科学
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DOI
PubMed
高影响因子
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