ANALYTICA CHIMICA ACTA
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2024
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IF 5.7
Hanqi Yang,Jingdong Peng,Huanjun Peng,Hanlin Zeng,Jiayu Yu,Jiajia Wu,Xiang Wang
Background Food safety has always been a great concern, and the detection of additives is vital to ensuring food safety. Therefore, there is a necessity to develop a method that can quickly and efficiently separate and detect additives in food. High performance liquid chromatography is widely used in the analysis and testing of food additives . Ionic liquids have attracted wide attention in the preparation of high performance liquid chromatography stationary phases owing to their high stability, low vapor pressure and adjustable structure. Results We developed a novel dicationic imidazole ionic liquid stationary phase for the simultaneous determination of organic preservatives (sodium benzoate, potassium sorbate) and inorganic preservatives (nitrate and nitrite) in foodstuffs under mixed-mode chromatography. The method had the advantages of easy operation, high reproducibility, good linearity and precision. In the detection of these four preservatives, the limit of detection ≤0.4740 mg⋅L −1 and the limit of quantification ≤1.5800 mg⋅L −1 . The intra-day and inter-day precision were less than 4.02%, and the recovery rate was 95.90∼100.19 %. At the same time, we also characterized the stationary phase, explored the mechanism and evaluated the chromatographic performance. The stationary phase was able to operate under the mixed mode of reversed phase/hydrophilic interaction/ion exchange chromatography, and it was capable of separating hydrophilic substances, hydrophobic substances, acids, and inorganic anionic substances with good separation efficiency and had high column efficiency. Significance In summary, the stationary phase has a promising application in the routine analysis of organic and inorganic preservatives in food. In addition, the stationary phase has good separation ability for hydrophilic, hydrophobic, ionic substances and complex samples, making it a prospective material for chromatographic separation.
研究领域:
分析化学
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食品安全
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色谱技术
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DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
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2025
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IF 4
Minyi Yuan,Zheng Zhao,Ji Wu,Sumin Bian,Yuling Liao,Ying Zhou,Huikai Shao,Zhengjin Jiang,Qiqin Wang
To meet the increasing demand for the separation of complex samples, a novel monolithic stationary phase with hydrophobic and hydrophilic functionalities was developed by using 3-(1-(4-vinylbenzyl)-1H-imidazol-3-ium) propane-1-sulfonate (VBIPS) as monomer, pentaerythritol triacrylate (PETA) as crosslinker. The optimized mixed-mode poly(VBIPS- co -PETA) monolith exhibited good mechanical strength, high permeability (K = 0.23 × 10 -14 m 2 in 100% ACN, 0.23 × 10 -14 m 2 in 100% MeOH, and 0.11 × 10 -14 m 2 in 100% H 2 O), and multiple interaction modes, including hydrophilic, hydrophobic, hydrogen, and electrostatic interactions. The highest column efficiency of 83,330 plates/m was achieved for thiourea at a linear velocity of 0.23 mm/s. Systematic evaluations confirmed strong retention and separation of polar substances (e.g., benzoic acids, nucleoside bases, phenols), primarily due to the sulfobetaine-derived hydrophilicity as well as effective separation of nonpolar substances (e.g., aniline, aryl ketones, polyaromatic hydroxy compounds), facilitated by π-π stacking interactions between analytes and benzene rings within the stationary phase. Overall, this zwitterionic imidazolium sulfonate-functionalized monolith successfully combines hydrophobic and hydrophilic groups in a single continuous bed, enabling efficient separation of both polar and nonpolar analytes under low backpressure. This work enriches the library of mixed-mode stationary phases, and broadens the detection scope for complex sample analysis.
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高影响因子
JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES
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2019
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IF 0.987
Yang-Fang He,Han-Qing Cai,Hong-Mei Zhang,Zhi-Hui Ren,Huan Tang,Yan Li,Xiao-Wei Zhou,Wen-Long Liu,Jin Pei,Shu-Ying Liu
In order to understand the significant differences in activities and effects between Asian ginseng (ASG) and American ginseng (AMG), it is important to study the correlation between chemical structures and biological activities in the two types of herbs. However, more attention has been paid to the analysis of ginsenosides in previous reports distinguishing between ASG and AMG. There are some other bioactive compounds besides ginsenosides, however, few studies have focused on a systematic comparison of these types of compounds. Two metabolomic methods were developed in this study by qualitative data acquisition using normal phase liquid chromatography mass spectrometry (NPLC-MS) and reverse phase liquid chromatography mass spectrometry (RPLC-MS) respectively, in combination with principal component analysis (PCA). Results show that both NPLC-MS and RPLC-MS-based metabolomic methods are feasible in composition profiling, biomarker screening as well as in discrimination of ASG and AMG. 17 ginsenosides were identified as analytical markers in RPLC-MS-based metabolomic method. In comparison, using NPLC-MS-based method, 5 ginsonosides, two amino acids as well as 1 oligosaccharide were identified as analytical markers. Therefore, RPLC-MS-based metabolomic method exhibits better profiling in ginsenosides, while NPLC-MS-based metabolomic method offers the advantage that multiple active ingredients can be determined simultaneously. The two methods are both helpful in identification of biomarker as well as in discrimination of American ginsengs from Asian ginsengs.
研究领域:
植物化学
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分析化学
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中药学
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DOI
高影响因子
Journal of Analysis and Testing
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2025
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IF 7
Li Han,Cui Yuanyuan,Zhen Changqing,Lin Xiaohui,Li Ke,Yang Chengxiong
Microporous organic network (MON) has emerged as efficient stationary phases for high-performance liquid chromatographic (HPLC) separation. Nevertheless, the inherent superhydrophobic networks made their applications limited in the reversed-phase (RP) mode. In this work, a novel amino acid L-cysteine (L-Cys) modified core-shelled microsphere MON@SiO 2 -L-Cys was synthesized via the efficient thiol-yne “click” reaction for hydrophilic interaction chromatography /reversed-phase liquid chromatography (HILIC/RPLC) mixed-mode chromatographic separation. Baseline separation of various hydrophilic and hydrophobic compounds including aromatic ketones, phthalate esters, alkylbenzenes, amines, polycyclic aromatic hydrocarbons, phenols, nucleosides, nucleic acid bases, sulfonamides, water-soluble vitamins, cephalosporin antibiotics, and estrogens was realized on MON@SiO 2 -L-Cys packed column based on the predesigned mixed-mode retention mechanisms. The MON@SiO 2 -L-Cys packed column also exhibited higher selectivity compared to bare SiO 2 , MON@SiO 2 without L-Cys, and C 18 packed columns, revealing the synergistic interactions of MON’s networks and the modified L-Cys molecules. This work provided a feasible way to construct a novel amphipathic MON-based stationary phase, broadened the application scope of MON for hydrophilic analytes, and uncovered the prospects of MON in mixed-mode HPLC.
研究领域:
分析化学
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材料科学
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高影响因子
JOURNAL OF CHROMATOGRAPHY A
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2024
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IF 3.8
Xiang Wang,Xingrui Wang,Hanqi Yang,Hanlin Zeng,Zhiqiang Xu,Wenhao Chen,Guangming Zhou,Jingdong Peng
In this study, we synthesized and employed an ionic gel-functionalized silica stationary phase for high-performance liquid chromatography. The successful fabrication of the stationary phase was confirmed through attenuated total reflection-Fourier transform infrared spectroscopy (ATR-FTIR), X-ray photoelectron spectroscopy (XPS), zeta-potential measurements, and elemental analysis (EA). Comparative performance evaluation against a commercial column demonstrated the prepared column's effectiveness in the mixed mode of reversed-phase liquid chromatography (RPLC), hydrophilic interaction liquid chromatography (HILIC), and ion chromatography (IC). Moreover, the stationary phase exhibited exceptional retention repeatability in per aqueous liquid chromatography, showcasing its potential as an environmentally friendly analytical method. Mechanistic investigations unveiled multiple solute-stationary phase interactions, including π-π interactions, hydrogen bonding, and ion exchange. Finally, we applied the developed stationary phase for the precise detection of preservatives in carbonated beverages and jelly, achieving high levels of accuracy and recovery rates.
研究领域:
分析化学
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环境科学
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食品科学
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DOI
PubMed
高影响因子
TALANTA
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2021
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IF 6.057
Jianzhong Wang,Jianshan Wang,Xiaohui Ning,Jiawei Liu,Hongjun Xia,Guangping Wan,Quan Bai
In this paper, a cysteine-functionalized zwitterionic stationary phase (Cys-silica) was prepared based on the “thiol-ene” click chemistry between cysteine and vinyl-functionalized silica, and was further modified with bromoethane, 1-bromooctane and 1-bromooctadecane, respectively, to obtain a series of quaternary ammoniation-functionalized stationary phases (Cys-silica-C n , n = 2, 8 and 18). These zwitterionic stationary phases were regarded as reversed-phase/ion-exchange (RP/IEC) mixed-mode chromatography (MMC) stationary phases for protein separation. The retention behaviors of proteins on these zwitterionic stationary phases were carefully investigated. The results indicated that the retentions of acidic and basic proteins on these zwitterinonic stationary phases were significantly influenced by the acetonitrile and salt concentrations, pH of mobile phase as well as the hydrophobicity of the ligand. The separation selectivity of proteins on these zwitterionic stationary phases strongly depended on the pH value of mobile phase. The baseline separation of 6 kinds of basic proteins can be achieved at pH 8.0 using Cys-silica-C2 or Cys-silica-C8 column, and 5 kinds of acidic proteins can also be separated completely at pH 4.0 with Cys-silica-C2 column. Moreover, owing to the quaternary ammoniation-functionalization on Cys-silica by using appropriately hydrophobic bromoalkanes , the selectivity and separation efficiency of proteins can be enhanced greatly. As a result, the acidic and basic proteins can be separated completely step by step from the complex sample by adjusting pH of mobile phase using a single Cys-silica-C2 column, which illustrates that the cysteine-functionalized zwitterionic stationary phase has a great potential for protein separation.
研究领域:
生物化学
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分析化学
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PubMed
高影响因子
FOOD CHEMISTRY
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2023
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IF 8.8
Liqi Ai,Lei Liu,Lin Zheng,Yang Liu,Baoguo Sun,Guowan Su,Jucai Xu,Yajun Chen,Mouming Zhao
Food-derived antioxidant peptides have become the focus of research due to their high safety and low cost. However, the discovery is suffering from a low efficient and empirical approach, involving multi-step off-line separation and identification. In this work, an on-line stop-flow RPLC × SEC -MS/DPPH radical scavenging activity analysis system was developed. For optimization, the conditions: 10 m reaction loop, 200 μM DPPH radical concentration, 40℃ temperature and 0.06 % formic acid were recommended. The system was fully validated by its application in glutathione analysis. The system was further applied in analysis of complex mixed standards, and the dipeptides GC (Gly-Cys) and CW (Cys-Trp) with relatively strong DPPH radical scavenging activity were validated. Maize protein hydrolysates were used for tests and the peptide AC (Ala-Cys) of high probability with strong DPPH radical scavenging activity was identified, demonstrating a high potential of the system. This would help to facilitate the discovery of antioxidative peptides in the future.
研究领域:
食品科学
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分析化学
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DOI
PubMed
高影响因子
TALANTA
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2024
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IF 5.6
Changwei Tang,Zilong Yang,Changle Li,Jiawei Liu,Quan Bai
The polymerization-induced colloid aggregation (PICA) method is commonly used to create SiO 2 @SiO 2 core–shell silica microspheres (CSSMs), but it often encounters challenges such as incomplete shell coating and poor reproducibility. In this paper, the formation mechanism of the silica shell layer during the preparation of SiO 2 @SiO 2 CSSMs using the PICA method was investigated. It was found that ureido modification can reduce the Zeta potential of the silica core surface, facilitating the deposition of coacervates formed by urea-formaldehyde resin (UF) and silica nanoparticles on the silica core surface to form the SiO 2 shell layer when the Zeta potential of the surface is in the range of −20.1 mV to −4.8 mV. By controlling the interfacial state and surface potential of the SiO 2 core, the issue of inconsistent reproducibility in preparing SiO 2 @SiO 2 CSSMs can be overcome. Furthermore, optimization of experimental parameters such as pH, reaction temperature, water content, and reaction time can enhance the formation process. The thickness of the shell and pore size of CSSMs can be successfully adjusted by varying the reaction time and the particle size of colloidal silica sol, respectively. With optimal conditions, the semi-scale production yield of SiO 2 @SiO 2 CSSMs can be increased to 50 g. The SiO 2 @SiO 2 CSSMs were modified with octadecyltrichlorosilane (ODS) to be used as stationary phases in reversed phase liquid chromatography (RPLC) for fast separation of small solutes, peptides, and proteins. The superior separation efficiency indicates that the improved PICA method has the potential to be utilized as an alternative to the layer-by-layer method for large-scale production of SiO 2 @SiO 2 CSSMs.
研究领域:
材料科学
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化学工程
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分析化学
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DOI
PubMed
高影响因子
TALANTA
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2019
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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
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色谱学
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DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
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2021
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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
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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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2023
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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
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色谱学
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PubMed
高影响因子
Acta Pharmaceutica Sinica B
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2024
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IF 14.7
Yutian Lei,Yuan Shen,Feng Chen,Rui He,Zhang Zhang,Ying Zhou,Jin-Chen Yu,Jacques Crommen,Zhengjin Jiang,Qiqin Wang
The dynamic tracking of antibody‒drug conjugates (ADCs) in serum is crucial. However, a versatile bioanalytical platform is lacking due to serious matrix interferences, the heterogeneity and complex biotransformation of ADCs, and the recognition deficiencies of traditional affinity technologies. To overcome this, a multiepitope recognition technology (MERT) was developed by simultaneously immobilizing CDR and non-CDR ligands onto MOF@AuNPs. MERT’s excellent specificity, ultrahigh ligand density, and potential synergistic recognition ability enable it to target the different key regions of ADCs to overcome the deficiencies of traditional technologies. The binding capacity of MERT for antibodies is ten to hundred times higher than that of the mono-epitope or Fc-specific affinity technologies. Since MERT can efficiently capture target ADCs from serum, a novel bioanalytical platform based on MERT and RPLC‒QTOF-MS has been developed to monitor the dynamic changes of ADCs in serum, including the fast changes of drug-to-antibody ratio from 3.67 to 0.22, the loss of payloads (maytansinol), and the unexpected hydrolysis of the succinimide ring of the linker, which will contribute to clarify the fate of ADCs and provide a theoretical basis for future design. In summary, the MERT-based versatile platform will open a new avenue for in-depth studies of ADCs in biological fluids.
研究领域:
药学
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生物分析化学
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生物技术
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药物递送系统
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DOI
PubMed
高影响因子