ANALYTICAL LETTERS
·
2022
·
IF 2.267
Xu-Feng Wang,Qiang Wang,Ying-Xia Zhang,Jin-Lan Yang,Dong-Hao Zhao
A sensitive and efficient magnetic amino modified multi-walled carbon nanotubes (m-MWCNT-NH2)-based magnetic dispersive solid-phase extraction (m-dSPE) coupled with hydrophilic interaction liquid chromatography–tandem mass spectrometry (HILIC-MS/MS) strategy is reported for the simultaneous determination of 13 paralytic shellfish toxins (PSTs) in bivalve mollusks. The samples were extracted twice with 1% acetic acid and purified using optimized m-dSPE procedures with Fe3O4 coated MWCNT-NH2 composites as magnetic adsorbents. The adsorbed PSTs on the m-MWCNT-NH2 adsorbents were separated using a Ni-coated neodymium magnet and subsequently eluted with 2 mL water–acetonitrile–acetic acid (80:20:1, v/v/v) and analyzed by HILIC-MS/MS. The correlation coefficients (r) of the targeted toxins obtained in matrix-matched external standard curves were from 0.997 to 0.999. The PSTs were acquired and quantified in the multiple reaction-monitoring mode and the limits of detection and quantitation in bivalve mollusks were 1.10 to 4.51 μg/kg and 3.67 to 13.5 μg/kg, respectively. Spiked recoveries at three concentrations in negative samples were from 73.4% to 92.5% with precision less than 10.6%. The method validation was in accordance with 2002/657/EC guidelines and method application in commercial bivalve mollusk samples. The developed method was rapid, convenient and economical for the determination of the targeted toxins.
研究领域:
分析化学
·
食品安全
·
毒理学
✓ 已验证
产品关联
DOI
高影响因子
TALANTA
·
2019
·
IF 4.916
Qiaohong Peng,Yue Wu,Hailin Cong,Youqing Shen,Khalid Mahmood,Bing Yu
In recent decades, ionic liquid-modified packing materials as stationary phases of high performance liquid chromatography (HPLC) have attracted widespread attention due to their comprehensive properties. In this work, monodisperse porous polymeric ionic liquid microspheres were directly prepared using a seeded emulsion polymerization method and applied as stationary phase of HPLC. The effects of porogen , monomer and crosslinker on the properties of porous P(IL-DVB) microspheres were investigated in detail. Porous P(IL-DVB) microspheres with good stability, monodispersity and relatively high specific surface area were selected as stationary phase to successfully separate benzene and its homologues, and nucleosides and alkaloids under reversed phase chromatography (RPLC) mode and hydrophilic interaction chromatography (HILIC) mode, respectively.
研究领域:
分析化学
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材料科学
·
色谱学
✓ 已验证
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2021
·
IF 4.759
Chunmiao Bo,Yan Li,Bin Liu,Zhuanhong Jia,Xiaojun Dai,Bolin Gong
A strategy is proposed to develop a stationary phase for hydrophilic interaction liquid chromatography (HILIC) using the synergistic effect of polyhedral oligomeric silsesquioxane (POSS) and copolymer brushes. Octahedral octa-aminopropylsisesquioxane (8NH 2 -POSS) was first bound to silica gel, followed by bromination to form a cubic initiator. Then, using acrylamide (AM) and dihydroxypropyl methacrylate (DPMA) as mixed monomers, surface initiated-atom transfer radical polymerization was conducted to prepare a stationary phase comprising cubic copolymer brushes with amide and diol groups. The characterization of the stationary phase confirmed the successful synthesis of Sil-NH 2 -POSS/Poly(AM- co -DPMA). The chromatographic properties were investigated using nucleosides, organic acids and β-agonists to find that our designed column has superior hydrophilic property, better separation performance compared with classical HILIC columns consisting of diol- or amino-modified silica. The systematic investigation of the retention mechanism and separation selectivity using various types of polar compounds revealed that Sil-NH 2 -POSS/Poly(AM- co -DPMA) follows a mixed-mode retention composed of HILIC and electrostatic interactions. Besides, it exhibits good column efficiency and stability. The role of 8NH 2 -POSS in the separation was evaluated by comparing the performance of Sil-NH 2 -POSS/Poly(AM- co -DPMA) and poly(AM- co -DPMA)-modified silica without 8NH 2 -POSS. In conclusion, our designed based on POSS and hydrophilic copolymer brushes can contribute to the development of HILIC separation materials with enhanced performance.
研究领域:
分析化学
·
材料科学
·
化学工程
✓ 已验证
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2021
·
IF 4.759
Chao Fan,Bei Liu,Hui Li,Kaijun Quan,Jia Chen,Hongdeng Qiu
In this work, three new mixed-mode stationary phases were prepared, based on different ratio of N-vinyl pyrrolidone (NVP) copolymerized together with undecylenic acid (UA) on silica microspheres surface without silanization, which named Sil@NVPUA series. The combination of NVP and UA rendered the Sil@NVPUA suitable for reversed-phase liquid chromatography (RPLC) and hydrophilic interaction liquid chromatography (HILIC), and shown excellent methyl, planar, isomers and ion selectivity. Five types of model analytes including eight polycyclic aromatic hydrocarbons, six alkylbenzenes, eight nucleosides and nucleobases, seven ginsenosides and five oxazolidinones can be well separated on this stationary phase. The preparation method of NVP and UA modified silica-based stationary phase is simple, and it also provides a new idea for the design of synthetic polymers to develop mixed-mode chromatography.
研究领域:
色谱学
·
分析化学
·
材料科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
TALANTA
·
2023
·
IF 6.1
Fei Wang,Fan Yang,Jiawei Liu,Quan Bai
This paper is a continuation of research into the retention behavior and mechanism of solutes in hydrophilic interaction chromatography (HILIC) using stoichiometric displacement theory (SDT). A HILIC/reversed-phase liquid chromatography (RPLC) dual-retention mechanism was studied in detail using a β -CD HILIC column. The retention behaviors of three groups of solutes with varying polarities were studied over the entire range of water concentrations in the mobile phase on the β -CD column, resulting in the formation of “U-shape” curves when lg k ’ was plotted against lg[H 2 O]. Additionally, the effect of hydrophobic distribution coefficient lg P O/W on the retention behaviors of solutes in HILIC and RPLC modes was also examined. A four-parameter equation derived from the SDT-R was found to accurately describe the “U-shaped” curves of solutes with RPLC/HILIC dual-retention mechanisms on β -CD column. The theoretical lg k ’ values of solutes calculated using the equation were found to be in agreement with their experimental values, with correlation coefficients greater than 0.99. This indicates that the four-parameter equation derived from SDT-R can effectively describe the retention behaviors of solutes over the entire range of water concentrations in the mobile phase in HILIC. As such, SDT can be used as a theoretical guide for the development of HILIC, including the exploration of new dual-function stationary phases to enhance separation efficiency.
研究领域:
分析化学
·
色谱学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
TALANTA
·
2019
·
IF 4.916
Yiqiong Chen,Xinyue Ding,Dandan Zhu,Xucong Lin,Zenghong Xie
Nonspecific adsorption is a challenge of specific recognition on aptamer-based affinity monoliths. Here, a novel highly hydrophilic polyhedral oligomeric silsesquioxane (POSS)-containing aptamer-based hybrid-silica affinity monolith with a good recognition nature was prepared and used for specific discrimination of ochratoxin A (OTA). A homogeneous polymerization mixture consisted of POSS chemicals, hydrophilic monomers and aptamer solution was directly polymerized via the “one-pot” method. Preparation and characterization of the resultant affinity monolith were studied in detail. A highly hydrophilic nature was obtained and the typical hydrophilic interaction liquid chromatography (HILIC) was observed when acetonitrile (ACN) content in mobile phase was 25%, which reached the highest hydrophilicity of POSS-based hybrid monoliths. By using OTA as model analyte, the nonspecific adsorption was effectively suppressed. The recovery of the analogue ochratoxin B (OTB) was only about 0.1% even if the content of OTB was 50 times more than OTA, which was much better than other POSS-containing monoliths and polar siloxane-based hybrid monoliths. Applied to beer samples, the adsorption of background materials was drastically resisted, and efficient recognition of OTA was obtained with the recoveries of 94.9–99.8%. Much less disturbance was observed than that occurred in hydrophobic POSS-based affinity monolith. It lights an attractive implement with high hydrophilicity and specificity for online selective recognition of OTA.
研究领域:
分析化学
·
食品科学
·
材料科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
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
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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
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细胞生物学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2022
·
IF 4.601
Yufeng Shen,Huiliang Geng,Feifang Zhang,Zongying Li,Bingcheng Yang
A polyethyleneimine (PEI)-functionalized polymer substrate polar stationary phase was prepared for hydrophilic interaction chromatography (HILIC) by grafting PEI onto poly(styrene-divinylbenzene) (PS-DVB) microspheres. The phase shows a U-shape retention profile and it exhibits typical hydrophilic characteristic when the organic solvent fraction in the mobile phase is > 60%. Hydrogen bonding, anion exchange, and hydrophobic interaction are involved in the retention mechanism. Good separation and unique selectivity for acidic, basic and neutral polar analytes were achieved. It showed extremely low column bleed (comparable to that of blank) under gradient elution mode (even to 50% fraction of water) and wide pH tollerance range (at least 1–13).
研究领域:
分析化学
·
色谱学
·
材料科学
✓ 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）