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Nanomaterials · 2023 ·Vol. 13 ·期 6 ·1111 · IF 5.3

Preparation and Characterization of Nano-Fe3O4 and Its Application for C18-Functionalized Magnetic Nanomaterials Used as Chromatographic Packing Materials

Wen-Xin Liu,Wei-Na Zhou,Shuang Song,Yong-Gang Zhao,Yin Lu

A new type of magnetic nanomaterial with Fe3O4as the core and organic polymer as the shell was synthesized by seed emulsion polymerization. This material not only overcomes the problem of insufficient mechanical strength of the organic polymer, it also solves the problem that Fe3O4is prone to oxidation and agglomeration. In order to make the particle size of Fe3O4meet the requirement of the seed, the solvothermal method was used to prepare Fe3O4. The effects of the reaction time, amount of solvent, pH value, and polyethylene glycol (PEG) on the particle size of Fe3O4were investigated. In addition, in order to accelerate the reaction rate, the feasibility of preparing Fe3O4by microwave was studied. The results showed that under the optimum conditions, the particle size of Fe3O4could reach 400 nm and had good magnetic properties. After three stages of oleic acid coating, seed emulsion polymerization, and C18 modification, the obtained C18-functionalized magnetic nanomaterials were used for the preparation of the chromatographic column. Under optimal conditions, stepwise elution significantly shortened the elution time of sulfamethyldiazine, sulfamethazine, sulfamethoxypyridazine, and sulfamethoxazole while still achieving a baseline separation.Keywords:solvothermal method;chromatographic packing materials;magnetic Fe3O4particles;C18-functionalized magnetic nanomaterials

CAS / MDL: 67-56-1 127-79-7
研究领域: 化学 · 材料科学 · 分析化学
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JOURNAL OF APPLIED POLYMER SCIENCE · 2022 ·Vol. 139 ·期 47 ·e53180 · IF 3.057

Preparation and chromatographic application of β-cyclodextrin modified poly (styrene-divinylbenzene) microspheres

Yue Wang,Zhipeng Fang,Adeel Ahmed,Qiubo Wang,Hailin Cong,Youqing Shen,Bing Yu

In order to better realize the separation of chiral enantiomers and prevent chiral compounds with toxic side effects from causing harm to human beings, porous microspheres were modified to improve their chromatographic separation performance. In this paper, in order to verify the chromatographic performance of porous polymer microspheres, the precise and controllable synthesis of poly (styrene-divinylbenzene) (PS-DVB) microspheres was realized based on the two-step swelling method. Then, the porous PS-DVB microspheres were sulfonated with concentrated sulfuric acid. The sulfonated microspheres were grafted with diazo resin (DR), and then the 3,5-dichlorobenzene isocyanate modified β -cyclodextrin ( β -CD-DCIPI) was bonded to the sulfonated PS-DVB microspheres by the DR. Finally, the bond inversion occurred after UV irradiation. We have successfully solved the toxic effect of traditional coupling agents by using the unique photo-crosslinking reaction of DR. This novel and environmentally friendly chromatographic packing can be used to separate chiral compounds. The results showed that all of the eight compounds (chlorpheniramine; ibuprofen; benzoin; 2-phenylcyclohexanone; trans-stilbene oxide; Cobalt [III] acetylacetonate; Hesperetin; DL-Mandelic acid) can be separated. It is worth noting that the modified microspheres can achieve good separation of chiral compounds with the concentration of 1 mg/ml in 3 min.

研究领域: 分析化学 · 材料科学 · 药物化学
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TALANTA · 2015 · IF 3.545

Preparation, characterization and application of a reversed phase liquid chromatography/hydrophilic interaction chromatography mixed-mode C18-DTT stationary phase

Qing Wang,Yao Long,Lin Yao,Li Xu,Zhi-Guo Shi,Lanying Xu

A mixed-mode chromatographic stationary phase , C18-DTT (dithiothreitol) silica (SiO 2 ) was prepared through “thiol-ene” click chemistry. The obtained material was characterized by fourier transform infrared spectroscope, nitrogen adsorption analysis and contact angle analysis. Chromatographic performance of the C18-DTT was systemically evaluated by studying the effect of acetonitrile content, pH, buffer concentration of the mobile phase and column temperature. It was demonstrated that the novel stationary phase possessed reversed phase liquid chromatography (RPLC)/hydrophilic interaction liquid chromatography (HILIC) mixed-mode property. The stop-flow test revealed that C18-DTT exhibited excellent compatibility with 100% aqueous mobile phase. Additionally, the stability and column-to-column reproducibility of the C18-DTT material were satisfactory, with relative standard deviations of retention factor of the tested analytes (verapamil, fenbufen , guanine , tetrandrine and nicotinic acid) in the range of 1.82–3.72% and 0.85–1.93%, respectively. Finally, the application of C18-DTT column was demonstrated in the separation of non-steroidal anti-inflammatory drugs, aromatic carboxylic acids , alkaloids, nucleo-analytes and polycyclic aromatic hydrocarbons . It had great resolving power in the analysis of various compounds in HILIC and RPLC chromatographic conditions and was a promising RPLC/HILIC mixed-mode stationary phase.

研究领域: 分析化学 · 材料科学
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CHEMICAL RESEARCH IN CHINESE UNIVERSITIES · 2014 ·Vol. 30 ·期 5 ·855-862 · IF 1.119

Synthesis of chlorogenic acid imprinted chromatographic packing by surface-initiated atom transfer radical polymerization and its application

Niu Yuling,Ma Meihua,Gong Yanru,Wang Yue,Gong Bolin

A novel chromatographic packing of chlorogenic acid(CGA) molecularly imprinted polymer(MIP) based on the 5.0 μm silica was prepared by surface initiated atom transfer radical polymerization(SI-ATRP) with 4-vinylpyridine(4-VP) as functional monomer, ethyl glycol dimethacrylate(EDMA) as cross-linker in the mixture of methanol and water(7:3, volume ratio) under mild reaction conditions. The characteristics of CGA MIP were investigated by elemental analysis, thermogravimetric analysis(TGA), Fourier transform infrared spectrometry(FTIR) and atomic force microscopy(AFM). The effects of some chromatographic conditions such as mobile phase composition and temperature on the retention time were investigated. The adsorption capacity of the stationary phase for compounds was determined by frontal chromatographic technique. The results show that Freundlich isotherm fits the experimental adsorption isotherm data better than Langmuir model does. The relatively high heterogeneity index values regressed with the Freundlich isotherm suggest the formation of fairly homogeneous MIP. Thermodynamic data(ΔΔ H and ΔΔ S ) obtained by van’t Hoff plots reveal an entropy-controlled separation. The CGA MIP column was shown to be successful for the separation and purification of chlorogenic acid from the extract of Honeysuckle.

研究领域: 分析化学 · 高分子化学 · 药物分离纯化 · 材料科学 · 色谱技术
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CHROMATOGRAPHIA · 2022 ·Vol. 85 ·期 4 ·365-371 · IF 2.213

One-Step Solvothermal Synthesis of Sub-2-µm Sea Urchin-Like TiO2 Microspheres for High-Performance Liquid Chromatography Stationary Phase

Mei Ling,Tang Hao,Wang Shuai,Guo Yong,Liang Xiaojing

Sub-2-µm sea-urchin-like TiO 2 microspheres were prepared through the one-step solvothermal method. Results of scanning electron microscopy (SEM) and transmission electron microscopy (TEM) show that there are a lot of nanorods coming out from the center of the TiO 2 microsphere, making it look like a sea urchin. The morphology and structure of these microspheres are very suitable for chromatographic packing. During the separation of inorganic anions on this new stationary phase, the retention mechanism is electrostatic interaction, and the pH of the mobile phase plays an important role in retention behaviors. With this new stationary phase for separation of organic anions and nucleobases, Lewis acid–base interaction is more outstanding, which can cause peak broadening and tail for larger conjugated structure compounds. The separation of aromatic hydrocarbons on this new stationary phase demonstrates that Lewis acid–base interaction has a favorable influence on the separation of electron-rich aromatic hydrocarbons under normal phase chromatographic conditions. Graphical abstract

研究领域: 化学 · 材料科学 · 分析化学
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