JOURNAL OF CHROMATOGRAPHY A
·
2024
·
IF 3.8
Yiran Xia,Lushuai Wang,Yang Liu,Jiawei Liu,Quan Bai
Covalent organic frameworks (COFs) show promise as a stationary phase in high performance liquid chromatography (HPLC). However, there are only a few COFs-based stationary phases developed for HPLC separation so far. Therefore, it is crucial to not only develop more varieties of COFs-type stationary phases for HPLC separation, but also to explore the retention mechanism of solutes on these stationary phases. In this paper, a new in-situ growth method was developed to prepare β -ketoenamine COF-TpPa-1@SiO 2 composite microspheres, using spherical silica as the core material and COF-TpPa-1 fabricated by covalent conjugation of 1,3,5-triformylphloroglucinol (Tp) and p -phenylenediamine (Pa-1) as the COF shells. The resulting microspheres exhibit uniform morphology, good monodispersity, large specific surface area, narrow size distribution, and high stability. Due to diverse functional groups in the structure of COF-TpPa-1, the microspheres can offer multiple interactions, such as hydrophobic, π-π stacking and electron-donor–acceptor (EDA) between COFs and analytes. As a result, the COF-TpPa-1@SiO 2 composite microspheres can be used as a mixed-mode stationary phase for HPLC separation. The chromatographic performance and retention mechanism of the COF-TpPa-1@SiO 2 packed column were investigated by separating polar and non-polar solutes, as well as isomers, in various HPLC modes, including reversed-phase liquid chromatography (RPLC), hydrophilic interaction chromatography (HILIC), and RPLC/HILIC mixed-mode chromatography. The results showed successful separation of non-polar alkylbenzene homologues, polycyclic aromatic hydrocarbons (PAHs), and polar amines and phenols in RPLC mode. The “U-shaped” curves of retention factor with the ACN concentration in mobile phase for four nucleobases indicated that the solute retention on the column followed a mixed mode mechanism of RPLC/HILIC. Compared to a traditional C18 column, the COF-TpPa-1@SiO 2 column exhibited superior separation efficiency, stability, repeatability and reproducibility in the separation of analytes with different polarities. The column enhanced the aromatic, shape and planar selectivity for PAHs and isomers through π-π interaction and improved the separation efficiency for electron-deficient compounds due to EDA effect. At last, the column was successfully used to separate and detect the residues of 5 phenylurea herbicides (PUHs) in soil. All these results indicate the potential of COFs for chromatography applications.
研究领域:
分析化学
·
材料科学
·
色谱学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2024
·Vol. 416
·期 28
·6621-6638
·
IF 3.8
Chen Chang,Zheng Ting,Chen Yang,Li Zegeng,Wu Huan
The preparation of cellular metabolomics samples and how to achieve comprehensive coverage of different polar metabolites in cell samples in the analysis pose a challenge for cellular metabolomics. In this study, we optimized a metabolomics protocol based on ultra-high-performance liquid chromatography high-resolution mass spectrometry (UPLC/HRMS) for the extraction and detection of metabolites in A549 cells and exploration of the intervention effect of Qi-Yu-San-Long decoction (QYSLD) on A549 cells. The results indicate that the lowest level of ATP leakage was observed when A549 cells were quenched under liquid nitrogen. MeOH/chloroform/H 2 O (1:2:1) extraction yielded more chromatographic peaks and excellent reproducibility, and the relative extraction efficiency of most target metabolites was also high. And we optimized the chromatographic separation conditions in both HILIC and RPLC modes, enabling comprehensive detection and analysis of metabolites with varying polarities. Then, we applied the optimized method to UPLC-Q-TOF/MS-based metabolomics of A549 cells to study the mechanism of QYSLD intervention in non-small cell lung cancer (NSCLC). The CCK-8, EdU staining, and cell cycle assay showed that QYSLD inhibited the proliferation of A549 cells by interfering with the cell cycle and blocking them in the G1 phase. A total of 36 differential metabolites associated with the antitumor effects of QYSLD on NSCLC were identified, mainly involving nicotinate and nicotinamide metabolism, sphingolipid metabolism, and glycerophospholipid metabolism. And western blotting confirmed that the change in 1-methylnicotinamide levels after QYSLD intervention was associated with the inhibition of nicotinamide N-methyltransferase expression in A549 cells. Graphical Abstract
研究领域:
癌症生物学
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药理学
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代谢组学
·
细胞生物学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MICROCHIMICA ACTA
·
2021
·Vol. 188
·期 12
·1-11
·
IF 5.833
Fan Fangbin,Lu Xiaofeng,Wang Shuai,Wang Licheng,Liang Xiaojing,Guo Yong
By introducing functional groups such as quaternary amine groups, sulfonic acid groups, triazine groups, and other mespore nanomaterials into the hydrogel, better separation effect of some organic framework materials has been obtained. Due to a reasonable design and preparation strategy, the hydrogel composite-modified silica can be used in the selective separation of various analytes such as pesticides, alkylbenzenes, polycyclic aromatic hydrocarbons, nucleosides/bases, benzoic acids, antibiotics, and carbohydrates. Through the exploration of chromatographic retention behavior, it is proved that the column can be used in mixed-mode liquid chromatography. The intra-day relative standard deviation for retention time of this new stationary phase is 0.12–0.16% ( n = 10), and the inter-day relative standard deviation is less than 0.39% ( n = 5). This new stationary phase can also be used for separation in complex samples. The limit of detection (LOD) for chlorotoluron in farm irrigation water is 0.21 µg/L and the linear range is 2–250 µg/L. After optimizing the chromatographic conditions, the highest efficiency of the hydrogel column in RPLC and HILIC modes has reached 32,400 plates/m (chlorobenzuron) and 41,300 plates/m (galactose). This new type of hydrogel composite is a porous network material with flexible functional design and simple preparation method and its application has been expanded in liquid chromatography separation successfully. Graphical abstract The hydrogel composed of triallyl cyanate cross-linking agent and 3-(2-(methacryloyloxy) ethyl) dimethylamine) propane-1-sulfonate (SBMA) monomer which were co-modified on the surface of mesoporous silica with MOF-919 for separation in mixed-mode liquid chromatography.
研究领域:
分析化学
·
材料科学
·
纳米技术
·
色谱学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）