JOURNAL OF CHROMATOGRAPHY A
·
2014
·
IF 4.258
Qi Liu,Junan Xiao,Jingang Yu,Yixi Xie,Xiaoqing Chen,Hua Yang
A long-neglected recycling high performance liquid chromatography (R-HPLC) strategy was adopted to improve the enantioseparation efficiency in this work. Taking intractable isoxazolidine mixtures as the example, two different R-HPLC methods including single-column and twin-column based strategy were applied to improve the enantioseparation efficiency. Under the optimized conditions, these two methods present distinct separation results: the conceptually simple and commonly used single-column based R-HPLC led to severe peak broadening and degraded separation efficiency; on the contrary, the enantioseparation was significantly improved by adopting the relatively complicated twin-column strategy. This observed difference might be mainly attributed to less peak spreading and sample mixing of the latter, as a result of avoiding redirecting the effluent back to LC pump.
研究领域:
分析化学
·
药物化学
✓ 已验证
DOI
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2017
·Vol. 40
·期 18
·3718-3724
·
IF 2.557
Xu Ling,Li Zou,Zilin Chen
A polymeric column that contains multiwalled carbon nanotubes-β-cyclodextrin composite was developed. The composite was wrapped into the poly(butyl methacrylate-ethylene dimethacrylate) monolith column (0.76 mm id and 10 cm in length). The column was then applied for the online solid-phase microextraction of psoralen and isopsoralen from Fructus Psoraleae. Following microextraction, the coumarins were quantified by high-performance liquid chromatography with C 18 separation column and UV detection. The effects of sample flow rate, sample volume, and pH value were optimized. The method showed low limits of detection (20 pg/mL, S/N = 3) for both psoralen and isopsoralen. Finally the method was successfully applied to the determination of psoralen and isopsoralen in spiked herb extracts and rat plasma where it gave recoveries that ranged between 93.2 and 102.1%. The empty hydrophobic cavities of β-cyclodextrin and the hydrophobicity of multiwalled carbon nanotubes provided specific extraction capability for psoralen and isopsoralen.
研究领域:
分析化学
·
药理学
✓ 已验证
DOI
高影响因子
ANALYTICA CHIMICA ACTA
·
2019
·
IF 5.256
Haixia Lyu,Haoran Sun,Yimen Zhu,Jun Wang,Zenghong Xie,Jinxia Li
In this study, a double-recognized aptamer-molecularly imprinted monolithic column (Apt-MIP monolithic column) was prepared by introducing both aptamer and MIP to reduce non-specific adsorption. Its preparation parameters such as the time of photo-initiation, the dosage of photo-initiator and the concentration of aptamer were investigated in detail. The recovery ratios of ochratoxin A (OTA) to ochratoxin B (OTB) on Apt-MIP monolithic column, Apt monolithic column and MIP monolithic column were 116.1, 40.8 and 69, respectively. Even if the concentration of OTB was 10 times that of OTA, the recovery of OTB was only about 2.9%. Applied to beer samples, the prepared Apt-MIP monolithic column drastically resisted background adsorption and the high-specificity recognition for OTA was obtained with the recoveries of 95.5–105.9%. This work provided a simple and effective method to selectively identify OTA from complex samples.
研究领域:
食品安全
·
分析化学
·
生物技术
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2023
·
IF 3
Chengjiang Zhang,Yuhuang Li,Hongmei Yuan,Zeyi Lu,Qi Zhang,Lirong Zhao
Covalent organic frameworks (COFs) are a burgeoning class of crystalline porous materials with unique properties and have been considered as a promising functional extraction medium in sample pretreatment. In this study, a new methacrylate-bonded COF (TpTh-MA) was well designed and synthesized via the aldehyde-amine condensation reaction, and the TpTh-MA was incorporated into poly (ethylene dimethacrylate) porous monolith by a facile polymerization reaction inside capillary to prepare a novel TpTh-MA monolithic column. The fabricated TpTh-MA monolithic column was characterized with scanning electron microscope, Fourier transform infrared spectrometer, X-ray diffraction, and N 2 adsorption–desorption experiments. Then, the homogeneous porous structure, good permeability and high mechanical stability of TpTh-MA monolithic column was used as separation and enrichment media of capillary microextraction, which was coupled with high-performance liquid chromatography fluorescence detection for online enrichment and analysis of trace estrogens. The main experimental parameters influencing the extraction efficiency were systematically investigated. The adsorption mechanism for three estrogens was also explored and discussed based on hydrophobic effect, π-π affinity and hydrogen bonding interaction, which contributed to its strong recognition affinity to target compounds. The enrichment factors of the TpTh-MA monolithic column micro extraction method for the three estrogens were 107–114, indicating a significant preconcentration ability. Under optimal conditions, a new online analysis method was developed and exhibited good sensitivity and wide linearity range of 0.25–100.0 µg·L -1 with a coefficient of determination ( R 2 ) higher than 0.9990 and a low limit of detection with 0.05–0.07 µg·L -1 . The method was successfully applied for online analysis of three estrogens of milk and shrimp samples and the recoveries obtained from spiking experiments were in range of 81.4–113% and 77.9–111%, with the relative standard deviations of 2.6–7.9% and 2.1–8.3% ( n = 5), respectively. The results revealed the great potential for the application of the COFs-bonded monolithic column in the field of sample pretreatment.
研究领域:
分析化学
·
材料科学
·
食品安全
✓ 已验证
产品关联
DOI
PubMed
高影响因子
TALANTA
·
2025
·
IF 6.1
Hui Bai,Yinan Zhao,Lei Chen
The inherent presence of structurally similar stereoisomers in natural products poses great challenges for chiral quality control in pharmaceutical and botanical industries, particularly in differentiating the pharmacological activity of high-purity enantiomers. Multi-column methods are commonly used to separate multiple pairs of enantiomeric components, serious impact on the separation efficiency. To address this issue, a star hydroxypropyl cyclodextrin polymer (Star-HPCD) mixed-mode ligand with higher selectivity was designed to achieve both chiral recognition and structural selectivity. Sil-Star-HPCD chiral stationary phase (Sil-Star-HPCD CSP) enabled the simultaneous separation of three pairs of quinoline alkaloid stereoisomers during a single chromatographic run with a separation factor (α) greater than 1.5, significantly improving the analytical efficiency. Compared with the linear polymer structures, the supramolecular structure formed by star-shaped polymer significantly reduces the steric hindrance and improves the ligand density, which provides a prerequisite for adequate chiral recognition. Complementary evidence from molecular simulations and chiral NMR revealed multiple interactions at the molecular level for this single-column separation results. This work establishes a new strategy for the preparation of functionalized chiral ligands through structural design, which facilitates efficient stereoisomer analysis and chiral quality control in natural products.
研究领域:
分析化学
·
药物化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2022
·
IF 4.601
Guizhen Liu,Yanan Du,Tao Fu,Ying Han,Lifeng Pan,Jingwu Kang
An approach for profiling protein-protein interactions by using affinity purification with capillary monolithic immobilized metal affinity chromatography column (cm-IMAC) in combination with label free quantitative proteomics was described in the present work. The cm-IMAC columns were prepared in a single step by copolymerization of the function monomer , namely ( S )-2,2′-((1-carboxy-5-(pent‑4-enamido)pentyl)azanediyl)diacetic acid which provide a nitrilotriacetate (NTA) moiety to form chelated complexation with Ni (II) ions, inside the fused silica capillaries. The His 6 -tagged bait protein can be easily immobilized on the cm-IMAC columns through the formation of chelating complexation with the NTA-Ni (II) functional groups of the matrix. The cm-IMAC columns were used to explore protein-protein interactions (PPIs) on a proteomic scale when combined with label-free proteomics. A known interaction pair of proteins, namely NDP52 (amino acid sequence 10–126) and NAP1 (33–75) as well as Bcl-2 family proteins were used for proof of concept. New interactors of Bcl-X L were identified and validated by co-immunoprecipitation.
研究领域:
生物化学
·
蛋白质组学
·
分子生物学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Inorganics
·
2025
·Vol. 13
·期 9
·296
·
IF 3
Ming Huang,Shunyan Ning,Juan Liu,Lifeng Chen,Mohammed F. Hamza,Yuezhou Wei
This work develops a novel phosphate-functionalized extraction resin (HEHEHP + Cyanex272)/SiO2-P via the vacuum impregnation method for efficient separation of light rare earth element impurities from lanthanum (La3+) in nitric medium through synergistic extraction. Batch experiments have demonstrated superior adsorption selectivity toward impurity ions over La3+in a pH 4 nitric acid solution. Column studies confirmed exceptional performance under ambient conditions, achieving a lanthanum treatment capacity of 120.6 mg/g and over 98% impurity removal, which surpasses most reported values. Notably, this purification process enables direct production of purified La3+solutions through a single-column system without desorption, significantly enhancing efficiency and reducing costs. Mechanistic insights revealed combined ion exchange and coordination interactions between metal ions and P-OH/P=O groups, corroborated by advanced characterization and density functional theory calculations. These findings indicate a higher binding affinity of light rare earth compared with La3+. This strategy provides a scalable approach for ultra-high-purity lanthanum compound production in advanced optical and electronic applications.
研究领域:
湿法冶金
·
稀土元素分离
·
材料科学
·
分离技术
·
环境化学
✓ 已验证
产品关联
DOI
高影响因子