JOURNAL OF CHROMATOGRAPHY A
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2021
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IF 4.759
Xinying Zheng,Yang Qin,Xiaobing Meng,Zhengyu Jin,Liuping Fan,Jinpeng Wang
In this work, we for the first time synthesized the polyethylene glycol (PEG) bonded silica gel via KH-560 as a silane coupling reagent for column chromatography by a solid/liquid surface continuous reaction method. The molecular interaction, structure, morphology, and thermostability was characterized by fourier transform infrared spectroscopy (FTIR), elemental analysis (EA), scanning electronic microscope (SEM) and thermogravimetric analysis (TGA). Given that PEG is capable to self-assemble with α-CD, the PEG bonded silica gel was used as packing of column chromatography to achieve the selective separation of α-cyclodextrin (α-CD) at room temperature and atmospheric pressure. The bonded silica gel column could realize the effective separation of α-CD in the enzymatic hydrolysis mixture, which provides support for industrial separation of α-CD.
研究领域:
化学
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材料科学
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分离技术
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DOI
PubMed
高影响因子
Journal of Analysis and Testing
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2022
·Vol. 7
·期 1
·8-15
·
IF 0
Wang Danni,Li Hui,Qiu Hongdeng,Chen Jia
In this paper, silicon quantum dots (SiQDs) with green fluorescence are synthesized by solvothermal reaction of 3-(2,3-epoxypropoxy)propyltrimethoxysilane (GPTMS) and ethylenediaminetetraacetic acid (EDTA), and then SiQDs are bonded to the surface of silica to obtain a new nano-on-micro stationary phase (SiO 2 -SiQDs) for reversed-phase chromatography. The successful preparation of SiO 2 -SiQDs stationary phase is demonstrated by a variety of characterizations, such as transmission electron microscopy, laser confocal microscopy, elemental analysis and Fourier infrared spectroscopy. In addition, the chromatographic performance of the prepared stationary phase is evaluated and it shows good separation performance for non-polar substances such as alkylbenzene, aniline and polycyclic aromatic hydrocarbons in reversed-phase liquid chromatography. It is also verified that the stationary phase has good methyl selectivity and shape selectivity. More interestingly, the separation of prednisolone and hydrocortisone isomers can also be achieved at a low ratio of organic solvents, indicating that this new stationary phase has a good application prospect in isomer separation.
研究领域:
分析化学
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材料科学
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产品关联
DOI
JOURNAL OF CHROMATOGRAPHY A
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2023
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IF 4.1
Jiayu Yu,Jingdong Peng,Huanjun Peng,Zilong Zhang,Kun Fan,Pan Luo,Jiajia Wu,Hanqi Yang,Hanlin Zeng,Xiang Wang
Three structurally similar silane reagents with different terminal groups were prepared and bonded to silica to obtain three structurally similar stationary phases (Sil-Ph-COOH, Sil-Phe and Sil-Ph-NH 2 ). The prepared stationary phases were characterized through elemental analysis (EA) and Fourier Transform Infrared Spectroscopy (FT-IR). These three stationary phases provided acceptable retention repeatability (relative standard deviations between 0.08% and 0.13%) and high column efficiency (7.3 × 10 4 plates/m for uridine on Sil-Phe). The retention behavior of the three columns was investigated under different chromatographic conditions including different mobile phase ratio, salt concentration, pH etc. The retention mechanisms were explored by linear solvation energy relationships and Van't Hoff plots. Applications in separation under reversed phase liquid chromatography (RPLC), hydrophilic interaction liquid chromatography (HILIC) and ion exchange chromatography (IEC) mode were investigated. The results showed that the retention capacity of the stationary phases with different terminal groups to the analytes is very different, especially for carboxylic acids, because the surface charges of amino groups and carboxyl groups under weakly acidic conditions produce different electrostatic effects with dissociated carboxylic acids. Finally, the Sil-Phe column was employed to detect ibuprofen extracted from pharmaceutical ibuprofen capsules and vitamins extracted from vitamin tablets.
研究领域:
分析化学
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色谱学
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DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
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2014
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IF 4.258
Liyun Ma,Si-Min Liu,Lin Yao,Li Xu
Cucurbit[7]uril (CB7), one host macromolecule, possesses a hydrophobic inner cavity and two identical hydrophilic carbonyl fringe portals, thus interacting with a variety of guest molecules through hydrophobic, hydrogen bonding and ion–dipole interactions. These characteristics make CB7 a good candidate as the stationary phase (SP) modifier in high performance liquid chromatography (HPLC). In the present work, CB7 was immobilized onto silica (CB7-SiO 2 ) by a sol–gel approach. The obtained CB7-SiO 2 was characterized by Fourier transform infrared spectroscopy, thermogravimetric analysis and elemental analysis. The chromatographic performance of CB7-SiO 2 was then studied in detail, in both reversed phase (RP) and hydrophilic interaction liquid chromatographic (HILIC) modes. For probe aromatic compounds and dyes, the typical RP behavior was observed, mainly due to the predominant hydrophobic interaction between the analytes and CB7-SiO 2 . For probe alkaloids, the “U-shape” curves were obtained; in the methanol-rich part, HILIC performance was obvious, probably owing to hydrogen bonding and ion–dipole interactions. Compared to bare SiO 2 SP, the stronger retention and different selectivity were observed on CB7-SiO 2 . The CB7-SiO 2 SP remained stable within at least 11,000 column volumes of the MP, revealing the satisfactory stability of it. The proposed method integrated the advantages of CB7 and sol–gel method provided a feasible way for the wider application of CBs in separation science.
研究领域:
分析化学
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分离科学
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DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
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2021
·
IF 4.759
Yunchao Zheng,Meijun Wan,Jingqiu Zhou,Qiurong Luo,Die Gao,Qifeng Fu,Jing Zeng,Fengjiao Zu,Lujun Wang
Covalent organic frameworks (COFs) have showed expected potential in chromatographic separation due to unique structure and excellent performance. Nowadays, COF materials applied as chromatographic stationary phases is still in its infancy. Here, we modified COF materials on silica using benzene-1,4,5-tetracarboxylic dianhydride (PMDA) and 1,3,5-tris-(4-aminophenyl)triazine (TAPT) monomers by one-pot synthetic method for performing mixed-mode function, named as SiO 2 @COF. Five characterization methods including thermogravimetric analysis (TGA), scanning electron microscopy (SEM), Fourier transform infrared spectrometry (FT-IR), elemental analysis (EA) and powder X-ray diffraction (XRD) verified the morphology, structure characteristics and physicochemical properties of the materials. SiO 2 @COF for performing the separation of polar and nonpolar analytes on high performance liquid chromatography (HPLC) achieved the desired results. Retention mechanisms of the constructed SiO 2 @COF were researched via observing the effects of mobile phase with retention times. Results exhibited that the prepared stationary phase can provide various interaction modes, including hydrophobic, hydrophilic, hydrogen bonding and π-π interactions. In conclusion, the prepared SiO 2 @COF stationary phase can execute mixed-mode separation abilities and show potential for complex samples analysis.
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
TALANTA
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2015
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IF 3.545
Xiaohua Zhou,Xiaole Li,Aijuan Cao,Qiao Lijun,Ajuan Yu,Shusheng Zhang,Yangjie Wu
A new stationary phase for high-performance liquid chromatography was prepared by covalently bonding N-ferrocenyl(benzoyl)amino-acid esters (L 1 ) onto silica gel using 3-aminopropyltriethoxysilane as coupling reagent. The structure of new material was characterized by infrared spectroscopy , elemental analysis and thermogravimetric analysis . The chromatographic behavior of the phase was illustrated in reversed-phase (RP) and normal-phase (NP) modes using polycyclic aromatic hydrocarbons (PAHs), aromatics positional isomers, amines, 5-nitroimidazoles, organophosphorus pesticides and phenols as probes. Multiple mechanisms including hydrophobic, hydrogen bonding , π–π, dipole–dipole, charge-transfer and acid–base equilibrium interactions are involved. Thus, multi-interaction mechanisms and mixed-mode separation of the new phase can very likely guarantee its excellent chromatographic performance for the analysis of complex samples. The L 1 AminoSil column was successfully employed for the analysis of organophosphorus pesticides in vegetable.
研究领域:
分析化学
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色谱技术
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DOI
高影响因子
TALANTA
·
2017
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IF 4.162
Beibei Yang,Tianpei Cai,Zhan Li,Ming Guan,Hongdeng Qiu
In this paper, deep eutectic solvents (DESs) were firstly used as new and green solvents for the preparation of polymer-grafted silica stationary phases. 1-Vinylimidazole and acrylic acid were homopolymerized and copolymerized on silica via surface radical chain-transfer reaction in the DESs. Three stationary phases including poly(1-vinylimidazole)-, poly(acrylic acid)-, poly(1-vinylimidazole-co-acrylic acid)-grafted silica were obtained and characterized by elemental analysis and Fourier transform infrared spectroscopy. Their hydrophilic interaction chromatographic properties were investigated for separation of nucleosides , nucleobases, saccharides and amino acids . The retention changes of nucleosides and nucleobases on these columns were investigated under different chromatographic conditions including acetonitrile content, salt concentration, pH of mobile phase and column temperature. The repeatability of these columns was also investigated. The results demonstrate that DESs can be used as new media for the synthesis of silica-based stationary phases by homopolymerization and copolymerization on the surface of porous silica particles.
研究领域:
分析化学
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材料科学
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DOI
高影响因子
TALANTA
·
2014
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IF 3.511
Kai Hu,Suxiang Feng,Mingxia Wu,Shuang Wang,Wenjie Zhao,Qiong Jiang,Ajuan Yu,Shusheng Zhang
A new stationary phase for high-performance liquid chromatography was prepared by covalently bonding a V-shape cage heteroatom-bridged calixarene onto silica gel using 3-aminopropyltriethoxysilane as coupling reagent. The structure of the new material was characterized by infrared spectroscopy , elemental analysis and thermogravimetric analysis . Linear solvation energy relationship method was successfully employed to evaluate the new phase with a set of 34 solutes. The retention characteristic of the new phase shows significant similarities with ODS, as well as distinctive features. Multiple mechanisms including hydrophobic, hydrogen bonding , π–π and n–π interaction are involved. The chromatographic behavior of the phase was illustrated by using alkylbenzenes , aromatics positional isomers and flavonoids as probes. Moreover, inorganic anions were individually separated in anion-exchange mode by using the same column. Thus, multi-interaction mechanisms and mixed-mode separation of the new phase can very likely guarantee its excellent chromatographic performance for the analysis of complex samples. The column has been successfully employed for the analysis of clenbuterol in animal urine, and it is demonstrated to be suitable and a competitive alternative analytical method for the determination of clenbuterol.
研究领域:
分析化学
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药物分析
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产品关联
DOI
PubMed
高影响因子
TALANTA
·
2014
·
IF 3.511
Wei Yin,Huihui Chai,Renhua Liu,Changhu Chu,John A. Palasota,Xiaohui Cai
Iminodiacetic acid (IDA) is dicarboxylic acid amine, which may produce stronger interaction with polar or charged compounds than bidentate α,β-amino acid. In this article, a novel type of tridentate zwitterionic HILIC stationary phase was prepared by covalently bonding N-benzyl IDA on silica gel via copper( I ) catalyzed Huisgen azide-alkyne 1,3-dipolar cycloaddition (CuAAC). The structure of this stationary phase and all related intermediates was confirmed by NMR, FT-IR, MS spectrum and elemental analysis . The new stationary phase showed good HILIC characteristics and high column efficiency (the theoretical plate number is up to 44000 plates m −1 in the case of guanosine) in the application of separation of polar compounds, including organic acids , organic bases, as well as highly polar and hydrophilic compounds, such as cephalosporins and carbapenems . Most of them displayed good peak shape and selectivity.
研究领域:
分析化学
·
色谱技术
✓ 已验证
产品关联
DOI
PubMed
高影响因子
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