JOURNAL OF CHROMATOGRAPHIC SCIENCE
·
2017
·Vol. 55
·期 6
·662-668
·
IF 0.984
Ma Xiaowei,Feng Fan,Yang Yang,Dang Xueping,Huang Jianlin,Chen Huaixia
Fe3O4@MIL-100 (MIL, Material Institut Lavoisier) core–shell magnetic microspheres were prepared and applied as the sorbent for the magnetic solid phase extraction (MSPE) of N,N-diethyl-m-toluamide (DEET) in baby toilet water for the first time. The synthesized magnetic metal–organic frameworks were characterized by transmission electron microscope, infrared spectroscopy and thermogravimetric analysis. The functionalized magnetic microparticles showed excellent dispersibility in aqueous solution. The MSPE conditions were investigated in detail. Under the optimized conditions, an MSPE–high performance liquid chromatography method for the determination of DEET was developed. The method was linear in the concentration range from 5 to 500 μg L−1 for DEET in baby toilet water and good linearity (r2 > 0.9998) was obtained for the calibration curve. The limit of detection was 1.5 μg L−1. Both the intra-day and inter-day precisions (relative standard deviations) were <3%.
研究领域:
分析化学
·
环境科学
·
材料科学
✓ 已验证
DOI
PubMed
高影响因子
ANALYTICAL CHEMISTRY
·
2026
·
IF 7.3
Simeng Yan,Xindan Zheng,Jiawei Liu,Quan Bai
Chiral covalent organic frameworks (CCOFs) have potential application in enantioseparation due to their advantages, such as large surface area, abundant chiral recognition sites, and good chemical stability in organic solvents. However, due to the lack of essential active groups in COFs structures, it is challenging to introduce chiral ligands, which poses a challenge to the preparation and promotion of CCOFs. In this study, a strategy was developed to prepare CCOF@SiO2 core–shell microspheres for enantioseparation using the Ugi and click reactions. Imine-linked COF@SiO2 core–shell microspheres were synthesized in situ by using nonporous silica microspheres as the core and TAPB-DMTP-COF as the COF shell. This shell was formed by covalently conjugating 1,3,5-tris(4-aminophenyl)benzene (TAPB) and 2,5-dimethoxyterephthalaldehyde (DMTP). The carbon–carbon double bond was introduced into the COF framework through the Ugi multicomponent reaction in the presence of 4-pentenoic acid and cyclohexene isocyanate. The olefin-linked Ugi-COF@SiO2 microspheres were then reacted with thiolated chiral ligands such as β-CD-SH, captopril, and l-cysteine to produce CCOF@SiO2 core–shell microspheres via the “thiol–ene” click reaction. These CCOF@SiO2 microspheres were used as stationary phases to separate various racemic compounds in the normal phase and reversed-phase liquid chromatography modes. The columns with different chiral ligands showed excellent chiral recognition and separation capabilities for chiral compounds with good reproducibility. The successful applications highlight the potential of using the Ugi and “thiol–ene” click reactions to incorporate double bond active groups and different chiral ligands into the imine-linked COFs framework. This study’s proposed strategy is versatile and offers a broad platform for the preparation and applications of CCOFs in enantioseparation.
✓ 已验证
产品关联
DOI
高影响因子
Chemical Engineering Journal Advances
·
2026
·
IF 6.9
Chaoying Zhang,Bohao Qi,Xin Hu,Jincheng Li,Yingchun Mu,Huan Liu
Sensitive determination of multiclass veterinary drug residues in aquaculture water requires efficient sample preparation capable of handling trace contaminants while minimizing sample consumption and manual operation. Here, a periodic magnetic actuation-assisted microfluidic enrichment platform was integrated online with HPLC–MS/MS for the determination of quinolones, sulfonamides, tetracyclines, and malachite green. Fe₃O₄@GO was magnetically confined within a multi-serpentine microchannel, and the effects of channel geometry and magnetic operating conditions on sorbent retention and flow-through capture were systematically evaluated. The multi-serpentine configuration limited Fe₃O₄@GO loss to 3.82% after ten operating cycles, while 200 mT and 10 Hz provided effective magnetic confinement and capture performance. In the final workflow, 50 μL of sample was loaded at 5 μL min⁻¹ for 10 min, followed by mobile-phase-mediated release and transfer through an online C 18 cleanup/trapping column for chromatographic analysis. The method achieved limits of detection of 0.02–0.17 μg L⁻¹, limits of quantification of 0.07–0.53 μg L⁻¹, recoveries of 79.84–97.66% in spiked real aquaculture water, and RSDs of 3.41–7.24%. These results demonstrate a low-volume and integrated sample-preparation strategy for multiclass veterinary drug determination in aquaculture-water matrices.
✓ 已验证
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2026
·
IF 2.5
Meng-Chao Wen,Ji-Yue Li,QianQian Sun,Chen Hu,SuLan Ju,Fang Tian,BiQing Chen,ChenYao Li,YanMei Liu,Jin-Yong Zhou,Jun Dong
Network pharmacological analysis of RGG was performed based on HPLC-Q-TOF-MS/MS. • RGG alleviates liver fibrosis and suppresses hepatic stellate cell activation. • RGG exerts anti-fibrotic effects through autophagy mediated by the PTEN/AKT/mTOR signaling pathway. To clarify the bioactive constituents and anti-fibrotic mechanisms of Rougan Granules (RGG), this study utilized HPLC-Q-TOF-MS/MS to identify its chemical profile, followed by network pharmacology and molecular docking to explore potential targets. In vivo, RGG was administered at different doses to mice with carbon tetrachloride (CCl 4 )-induced liver fibrosis. The attenuation of liver injury by RGG was evaluated via serum biochemical profiling, histological staining, and western blot analysis. In vitro, platelet-derived growth factor-BB (PDGF-BB) was used to activate LX-2 cells, and the mechanisms of RGG in suppressing hepatic stellate cell (HSC) activation were validated via immunofluorescence and western blot. Furthermore, autophagic flux was monitored using laser scanning confocal microscopy in LX-2 cells transfected with mRFP1-EGFP-LC3B lentivirus. A total of 120 chemical constituents were identified, with network pharmacology analysis indicating that quercetin, genistein, and kaempferol might serve as the primary bioactive components of RGG. Functional enrichment analysis revealed that common targets were significantly enriched in the phosphoinositide 3-kinase/protein kinase B (PI3K/AKT) signaling pathway. Molecular docking confirmed that these key components exhibited stable binding affinities for phosphatase and tensin homolog (PTEN) and AKT1. Both in vivo and in vitro experiments validated that RGG upregulates PTEN expression to inhibit the AKT/mechanistic target of rapamycin (mTOR) signaling pathway. Furthermore, RGG was shown to exert anti-fibrotic effects by inducing HSC autophagy through the modulation of this pathway. These findings reveal that RGG attenuates liver fibrosis via PTEN/AKT/mTOR-mediated autophagy, supporting its therapeutic potential.
✓ 已验证
DOI
PubMed
高影响因子
Metabolites
·
2026
·Vol. 16
·期 7
·446
·
IF 4.5
Zhouwei Li,Hongfei Wei,Jiahui Wu,Qiyuan Yang,Jiemei Liang,Xiaoxun Wang,Li Li
Background/Objectives: This study aims to establish a systematic phytochemical characterization and quality evaluation method to systematically evaluate the influence of multiple factors on the chemical composition ofTaxillus chinensis, thereby providing a scientific basis for its development, utilization, and quality control standards. Methods: To ensure a targeted and representative metabolic screening, six representative batches covering the major geographical origins and host plants were selected for initial metabolomic profiling. An integrated analytical approach combining UPLC-MS/MS-based widely targeted metabolomics, HPLC fingerprinting, and multi-component quantitative analysis with multivariate statistical analysis was employed. Results: Significant quality variations were identified across the samples. Metabolomics results indicated that while chemical component types were qualitatively consistent across growth conditions, their contents varied significantly. Unique differential metabolites clustered according to specific geographical origins or host plants. KEGG pathway analysis revealed that geographical origin primarily regulated phenylpropanoid biosynthesis, whereas host differences mainly influenced flavonoid and monoterpenoid biosynthesis. Furthermore, HPLC fingerprinting of 20 batches demonstrated similarities greater than 0.9, with 15 common peaks determined. Based on their high relative abundance, differential significance across samples, and documented pharmacological relevance to the herb’s traditional efficacy, six bioactive components—gallic acid, catechin, epicatechin, hyperoside, isoquercitrin, and quercitrin—were identified and quantified. Notably, samples originating from Wuzhou exhibited the highest total content of these components. Consistent with PCA and HCA results, gallic acid, hyperoside, isoquercitrin, and quercitrin were identified as potential markers driving quality differences. Conclusions: This integrated approach allows for a systematic analytical screening ofTaxillus chinensis, clarifying chemical variations caused by environmental and biological factors, and supporting the standardization and comprehensive utilization of this medicinal plant.
✓ 已验证
DOI
高影响因子
JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES
·
2026
·
IF 1.1
Jianwei Wang,Xin Tian,Jun Zhang
Polyoxyethylene alkyl ether carboxylic acid (AEC) is a high-performance surfactant widely used in personal care and industrial applications. Existing analytical frameworks often struggle with low sensitivity and the inability to simultaneously quantify active ingredients alongside residual raw materials. This study describes the development and validation of an HPLC-ESI-MS method for the comprehensive characterization of AEC products. Chromatographic separation was achieved on an XBridge® C18 column using a mobile phase consisting of methanol and 25 mmol/L ammonium formate (containing 0.2% formic acid) (80:20, v/v). The method enables the accurate quantification of residual AEO and the semi-quantitative estimation of the key byproduct polyethylene glycol ether carboxylic acid (PEG-CH2COOH). For C12-14 AEO and PEG-CH2COOH, the LODs were 0.2 and 0.5 μg/mL, and the LOQs were 0.6 and 1.5 μg/mL, respectively. Excellent linearity was observed (r ≥ 0.998), with mean recoveries ranging from 95.9% to 106.0%. Furthermore, mass spectrometric characterization facilitated the structural elucidation of PEG-CH2COOH. Based on these analytical findings, potential formation pathways involve the covalent incorporation of carboxymethyl groups through the oxidation or carboxymethylation of PEG terminal hydroxyl groups. This method provides a critical analytical tool for the quality control, safety assessment, and formulation optimization of AEC products.
✓ 已验证
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2025
·
IF 4
Liang Qi,Xinting Zhang,Longjiang Li,Xilan Li,Xiangna Chang
Prolonged use of cosmetics containing banned fluoroquinolones can cause skin disorders and increase drug resistance. The QuEChERS method holds considerable application prospect in the pretreatment of cosmetic samples. Although octadecyl (C 18 )-bonded silica sorbent is commonly used as a QuEChERS clean-up material, the conventionally commercially available bulk C 18 sorbent is relatively costly and has a limited purification mechanism. In this study, using dendritic silica sphere (dSiO 2 ) as the substrate, and through the condensation reaction between cyanuric chloride (CNCl) and the amino group, a dNSiO 2 -CNCl-C 18 sorbent was synthesized. The sorbent was characterized using infrared spectroscopy, transmission electron microscopy, surface area and pore size analysis, and water contact angle measurements. The experimental results regarding the matrix removal from the model cosmetic lotion showed that dNSiO 2 -CNCl-C 18 exhibited a higher matrix removal efficiency compared to a commercial C 18 sorbent. Furthermore, a QuEChERS-HPLC-FLD method was developed using dNSiO 2 -CNCl-C 18 for the simultaneous detection of four fluoroquinolones, norfloxacin (NOR), pefloxacin (PEF), enrofloxacin (ENR), and difloxacin (DIF). The linear ranges were 0.10 to 100.0 μg L −1 for NOR and PEF, and 0.05 to 100.0 μg L −1 for ENR and DIF, with coefficient of determination exceeding 0.999. Satisfactory spiked recoveries for the lotion sample ranged from 91.5% to 107.0%, with intra-day and inter-day precision values not exceeding 7.6%. The established method was subsequently validated through its successful application in additional cream and emulsion samples. dNSiO 2 -CNCl-C 18 exhibits low synthesis costs and demonstrates promising potential for matrix purification in various complex samples, facilitating the rapid determination of target compounds.
✓ 已验证
产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2025
·
IF 9.8
Ying Li,Yu Zhang,Li Zhang,Jun Dang
The screening of enzyme inhibitors faces challenges such as low efficiency. In this study, a novel online HPLC-FLD/pancreatic lipase recognition system was developed for the first time. The optimal operating parameters were established as a flow rate of 1 mL/min, with excitation and emission wavelengths for pancreatic lipase set at 221 nm and 303 nm, respectively. The effectiveness of this system was validated using orlistat. Subsequently, this system was applied to Lycium ruthenicum , where two petunidin-based anthocyanins pancreatic lipase inhibitors were efficiently isolated using medium-pressure liquid chromatography. Molecular docking elucidated that compounds 1 and 2 interact with the serine residue of pancreatic lipase, exhibiting binding energies of −13.12 kcal/mol and −12.22 kcal/mol, respectively. Enzymatic assays showed that the half-maximal inhibitory concentrations of compounds 1 and 2 were 9.67 μM and 147.37 μM, respectively. These docking and inhibition results confirm the system for efficiently discovering pancreatic lipase inhibitors.
研究领域:
植物化学
·
分析化学
·
酶学
·
天然产物化学
·
药物发现
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MARINE POLLUTION BULLETIN
·
2019
·
IF 3.782
Dan Qin,Min Zhao,Jiangtao Wang,Ziru Lian
A simple, sensitive and effective method was developed and validated for selective adsorption and quantitation of norfloxacin (NFX) from marine sediments and seawater samples using the novel molecularly imprinted silica polymers as sorbents followed by high-performance liquid chromatographic analysis with diode array detection (HPLC-DAD). The imprinted particles were characterized by different techniques and the molecular recognition for NFX was also investigated. Several parameters affecting the extraction efficiency of molecularly imprinted solid-phase extraction (MISPE) process were optimized. Three sediment and seawater samples from Weihai bay in China were analyzed and the results show that satisfactory recoveries (77.2–98.7%) were achieved in seawater samples with low relative standard deviation (RSD) values less than 6.89% (n = 3), and the recoveries in sediments were in the range of 75.5–91.7%. The limits of detection are respectivley 2 μg L −1 in seawater samples and 5 μg kg −1 in sediments.
研究领域:
环境科学
·
分析化学
✓ 已验证
DOI
高影响因子
CHROMATOGRAPHIA
·
2014
·Vol. 77
·期 23
·1653-1660
·
IF 1.37
Lv Tao,Zhao Xian-En,Zhu Shuyun,Ji Zhongyin,Chen Guang,Sun Zhiwei,Song Cuihua,You Jinmao,Suo Yourui
A novel hyphenated technique based on ultrasonic-assisted dispersive liquid–liquid microextraction (UA-DLLME) coupled with derivatization has been established for the determination of brassinolide (BL, a representative of brassinosteroids) by HPLC fluorescence detection. 9-Phenanthreneboronic acid is used as labeling reagent of BL. UA-DLLME parameters containing type and volume of extraction and disperser solvent, pH and ultrasonication time are optimized. Derivatization parameters are optimized included amount of 9-phenanthreneboronic acid, volume ratio of pyridine, derivatization time and temperature. Under optimal conditions, quantitative linear range of BL is 50–1,000 ng L −1 and excellent linear response is observed with correlation coefficient of 0.9996. Limit of detection and limit of quantification are calculated as 8.0 and 25.0 ng L −1 , respectively. RSDs of retention time and peak area are in the range of 0.68–0.97 % and 4.61–6.54 % for intra-day precision, 1.32–1.94 % and 7.28–9.75 % for inter-day precision, respectively. Accuracy is satisfactory in the range of 82.3–125.1 %. RSDs’ values of repeatability are in the range of 0.82–1.79 and 3.95–8.53 % for retention time and peak area, respectively. Enrichment factor for BL is 189. The results of recovery and matrix effect are in the range of 82.0–108.6 and 90.0–115.3 %, respectively. The proposed method has been applied for the determination of BL in Arabidopsis thaliana , Daucus carota and Brassica campestris L. leaves with much higher sensitivity than many other methods.
研究领域:
植物学
·
分析化学
✓ 已验证
DOI
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2012
·Vol. 36
·期 4
·789-795
·
IF 2.733
Ke-Jing Huang,Jing Li,Yan-Ming Liu,Lan Wang
The graphene functionalized with (3-aminopropyl) triethoxysilane was synthesized by a simple hydrothermal reaction and applied as SPE sorbents to extract trace polycyclic aromatic hydrocarbons (PAHs) from environmental water samples. These sorbents possess high adsorption capacity and extraction efficiency due to strong adsorption ability of carbon materials and large specific surface area of nanoparticles, and only 10 mg of sorbents are required to extract PAHs from 100 mL water samples. Several condition parameters, such as eluent and its volume, adsorbent amount, sample volume, sample pH, and sample flow rate, were optimized to achieve good sensitivity and precision. Under the optimized extraction conditions, the method showed good linearity in the range of 1–100 μg/L, repeatability of the extraction (the RSDs were between 1.8 and 2.9%, n = 6), and satisfactory detection limits of 0.029–0.1 μg/L. The recoveries of PAHs spiked in environmental water samples ranged from 84.6 to 109.5%. All these results demonstrated that this new SPE technique was a viable alternative to conventional enrichment techniques for the extraction and analysis of PAHs in complex samples.
研究领域:
分析化学
·
环境科学
✓ 已验证
DOI
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2019
·Vol. 42
·期 5
·1058-1066
·
IF 2.516
Yingying Feng,Xiaopeng Hu,Faqiong Zhao,Baizhao Zeng
A novel magnetic adsorbent Fe 3 O 4 /reduced graphene oxide-carbon nanotubes, was prepared by one-pot solvothermal synthesis method. It was characterized by scanning electron microscopy, X-ray powder diffraction and vibrating sample magnetometry. The diameter of Fe 3 O 4 microparticles was about 350 nm, which were covered by carbon nanotubes and reduced graphene oxide sheets, while carbon nanotubes inserted between the reduced graphene oxide sheets effectively prevented their aggregation. The composite had large surface area and good magnetic property, suiting for magnetic solid-phase extraction and the determination of sulfonamides, by coupling with high-performance liquid chromatography. Under the optimized conditions (including extraction time, amount of adsorbent, solution pH, ionic strength and desorption conditions), a good linear was achieved in the concentration range of 5–500 μg/L and the low limits of detection and low limits of quantification were 0.35–1.32 and 1.16–4.40 μg/L, respectively. The enrichment factors were estimated to be 24.72 to 30.15 fold. The proposed method was applied for the detection of sulfonamides in milk sample and the recoveries were 88.4–105.9%, with relative standard deviations of 0.74–5.38%.
研究领域:
分析化学
·
材料科学
·
食品安全
✓ 已验证
DOI
高影响因子
危险品化学品经营许可证（带存储）