MICROCHEMICAL JOURNAL
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2024
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IF 4.9
Yaqin Nan,Pingyi Zheng,Xiaoqian Yuan,Xinyu Xu,Xiao Zhang,Youxin Li
In this study, sulfopropyl ether β-cyclodextrin polymer (SPE-β-CDP) with simple synthesis steps using cheap reagents was large-scalely prepared. Characterization results showed the average sulfonic group substitution in each β-CD molecule was about 7.261, and there were 195.87 μmol/g β-CD units in polymer. It was low viscosity and produced a little effect on column pressure. It was used as chiral selectors first time to add into mobile phase to separate 13 chiral drugs in HPLC. After investigation, results showed buffer pH, chiral additive concentration, organic phase proportion in mobile phase and flow rate could affect chiral separation. High separation ability of SPE-β-CDP was proved through baseline separation of 12 drugs which attributed to the homogeneity of SPE-β-CDP in sulfonic acid group substitution degree and position. The resolutions of salbutamol, bisoprolol, chlorpheniramine, propranolol and metoprolol could be even up to 7.47–19.02, which were significantly better than that of some references. Separations of 4 chiral drugs were even better than that of CE. Compared with monomer, SPE-β-CDP showed better chiral separation ability. SPE-β-CDP could be used in both of C8 and C18 columns. It was stable in batches and showed good recyclability and reusability. These provided a new strategy for chiral separation.
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INDUSTRIAL CROPS AND PRODUCTS
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2024
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IF 5.6
Weikang Shen,Haobo Wang,Zhouzhe Lan,Guangzhi Xu,Qinxue Ni,Qiufen Mo,Youzuo Zhang,Yan Wang
Gardenia fruit oil (GFO) is a new emerging edible woody oil with few investigations of its’ refinement process. In this study, different degumming, deacidification and bleaching technologies were introduced for realizing moderate refining of the GFO based on the preservation of bioactive micronutrients. Firstly, a simple multi-stage solid phase extraction (SPE) combined with a lab- affordable HPLC-UV instrument was developed for determinations of several vital biological constituents, such as crocetin, geniposide, polyphenols, phytosterols and squalene in the GFO. Satisfactory limit of detection (LOD), limit of quantification (LOQ), recovery, intra-day and inter-day precision were obtained. Subsequently, changes of those phytochemicals during three types of degumming, followed by three kinds of deacidification and then three ways of bleaching were investigated, offering insightful suggestions for achieving moderate refining of the GFO. Finally, the refined GFO might be suggested as a potential functional edible oil with valuable micronutrients. To our knowledge, this is the first study investigating moderate refinement techniques for GFO, as well as developing novel methods for phytonutrients analysis in the GFO.
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MOLECULES
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2019
·Vol. 24
·期 15
·2705
·
IF 3.06
Feng Li,Sen Guo,Shanshan Zhang,Sainan Peng,Wei Cao,Chi-Tang Ho,Naisheng Bai
Bee pollen contains all the essential amino acids needed by humans. China is the largest producer of bee pollen in the world. In the present study, we identified 11 fatty acids inF. esculentumbee pollen oil by GC-MS analysis, and 16 compounds were isolated fromF. esculentumbee pollen by column chromatography and identified. A high-performance liquid chromatography-diode array detector (HPLC-DAD) method was established for the quality control ofF. esculentumbee pollen. A validated HPLC-DAD method was successfully applied to the simultaneous characterization and quantification of nine main constituents in seven samples collected from seven different areas in China. The results showed that all standard calibration curves exhibited good linearity (R2> 0.999) in HPLC-DAD analysis with excellent precision, repeatability and stability. The total amount in the samples from the seven regions ranged from 23.50 to 46.05 mg/g. In addition, seven compounds were studied for their bioactivity using enzymic methods, whereby kaempferol (3) showed high α-glucosidase inhibitory activity (IC50: 80.35 μg/mL), ergosterol peroxide (8) showed high tyrosinase inhibitory activity (IC50: 202.37 μg/mL), and luteolin (1) had strong acetylcholinesterase inhibitory activity (IC50: 476.25 μg/mL). All results indicated thatF. esculentumbee pollen could be a nutritious health food.Keywords:bee pollen;enzyme inhibitory activity;HPLC-DAD;GC-MS;quality analysis
研究领域:
植物化学
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食品科学
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药理学
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FOOD CHEMISTRY
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2017
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IF 4.529
Yue Zhao,Ying Wang,Zi-Tao Jiang,Rong Li
An off-line high performance liquid chromatography (HPLC) coupled with chemical methods has been developed to evaluate antioxidant activity of 11 standard polyphenol compounds (SPCs) and vitamin C (Vc) in terms of radical scavenging abilities. The structure–activity relationships of each SPC were also discussed. SPCs showed different abilities in scavenging 2,2-diphenyl-1-picrylhydrazyl (DPPH ), 2,2′-azinobis-3-ethyl-benzthiazoline-6-sulphonate (ABTS + ) and hydroxyl ( OH) free radicals. Among SPCs, quercetin and kaempferol, as typical flavonoids, displayed the greatest radical-scavenging activities and even exhibited higher activity in OH radical removal ability than that of Vc. Furthermore, the proposed method was also applied to screening polyphenolic antioxidant components from Cichorium endivia L. ( C. endivia ) seed extract. The results indicated that cynarin in the extract was a more active compound to scavenge DPPH and ABTS + radicals than chlorogenic acid, while chlorogenic acid had stronger capacity in scavenging OH free radicals.
研究领域:
分析化学
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植物化学
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JOURNAL OF MOLECULAR LIQUIDS
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2020
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IF 5.065
Qilong Xie,Ming Xia,Huaiqian Lu,Hui Shi,Dekui Sun,Bo Hou,Litao Jia,Debao Li
A sample preparation method for the extraction of bisphenol A (BPA) from edible oils was established via simple, green, and sensitive deep eutectic solvent-based liquid-liquid microextraction (DES-LLME) before high-performance liquid chromatography (HPLC) with diode array detector (DAD). The deep eutectic solvent (DES) formed by tetrabutylammonium bromide (TBAB) and methanol was acted as the extractant. All parameters in the DES-LLME step, including the type and volume of extractants, the extraction time, and centrifugation time, were investigated and optimized. The application of hydrophilic DES in oils expands the selection of LLME extractants. Under the optimized conditions, the calibration curves in the range of 10–500 ng g −1 with a correlation coefficient of r > 0.999, and the detection limit was 0.8 ng g −1 . The relative standard deviations of intra-day and inter-day repeatability were 4.3% and 6.2%, respectively, and the recoveries varied between 88.7% and 97.3%. This developed method was successfully employed for measuring BPA in 6 edible oil samples.
研究领域:
分析化学
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环境科学
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食品安全
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JOURNAL OF HAZARDOUS MATERIALS
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2026
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IF 10.6
Fenghong Wei,Pei Wang,Junjun Hu,Yanping Zheng,Xiaojia Huang
Sample preparation is critical in developing a sensitive and accurate method for the monitoring of ultrashort- to long-chain perfluorocarboxylic acids (PFCAs) in complex samples. However, it remains a formidable challenge in the simultaneous and efficient extraction of ultrashort- to long-chain PFCAs (U-L@PFCAs) due to their significantly different polarity. In this connection, the electric field-assisted microextraction (EFAM) was introduced for the first time to efficiently co-extract ultrashort- to long-chain species. According to the chemical properties of the studied U-L@PFCAs, a new microelectrode based on a monolithic adsorbent (MEMA) was tailored using diallylamine and 1,1,1,3,3,3-hexafluoroisopropyl acrylate as dual monomers and employed as the microelectrode of EFAM. Results disclosed that the application of opposite directions and different intensities of electric field at adsorption and desorption stages enhanced the increase of extraction efficiencies by 78.6–131% in comparison with the omission of electric field. In addition, the adsorption characteristics, behavior, and mechanism of MEMA@EFAM towards the investigated U-L@PFCAs were explored. Under the selected microextraction conditions, a sensitive and reliable method based on an isotope internal standard calibration curve technique for monitoring ultra-trace U-L@PFCAs in various environmental water and human urine samples was established by combining MEMA@EFAM with HPLC-MS/MS detection. Low detection limits of 0.13–1.4 ng/L and superior precision (RSDs varied from 2.8% to 9.1%) were achieved with minimum background interference. The present study provides a highly competitive alternative for the broad-spectrum monitoring of PFCAs.
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MICROCHEMICAL JOURNAL
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2026
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IF 5.2
Yaxin Liu,Ruiyang Ma,Weihua Liu,Le Zhang,Yaxing Guo,Qiuhua Wu,Zhi Wang
A new porous BPM-HCP with tunable hydrophobicity was designed and prepared. • It proved to have an excellent adsorption capability for nitroimidazoles (NIIMs). • Adsorption is driven by π-stacking and balanced hydrophilic/hydrophobic interaction. • A SPE-HPLC method was developed for the detection of NIIMs in complex matrices. • The method is effective and can satisfy the determination of NIIMs in food samples. A benzyl-bis(diphenylphosphine)-based hyper crosslinked polymer (denoted as BPM-HCP) was fabricated with the use of α,α’-dichloro- p -xylene as cross-linker and bis(diphenylphosphino)methane as monomer. The characterization of the polymer was made and subsequently it was explored as an adsorbent for solid-phase extraction (SPE) of nitroimidazoles (NIIMs). The key experimental parameters that affect the extraction efficiency were investigated and optimized. BPM-HCP demonstrated high capability for the effective extraction of trace NIIMs from water, chicken meat and beef samples. Its superior and selective enrichment capability could be attributed to multiple mechanisms: electrostatic attraction, π-stacking, hydrogen bonding, and hydrophobic interactions. Following SPE, the extract was analyzed by HPLC-UV. After optimization, the method for the determination of NIIMs in environmental water, chicken meat and beef samples produced good linear responses within the concentration ranges of 0.21–120.0 ng mL −1 , 3.75–120.0 ng g −1 , and 2.43–200.0 ng g −1 , respectively, with the correlation coefficients ( r ) falling in the range of 0.9905–0.9997. The limits of detection ranged from 0.025 to 0.067 ng mL −1 for water, 0.625–1.250 ng g −1 for chicken, and 0.53–0.81 ng g −1 for beef. The quantification limits were 0.08–0.21 ng mL −1 (water), 1.88–3.75 ng g −1 (chicken), and 1.59–2.43 ng g −1 (beef), depending on compounds. The recoveries of the method for all the samples ranged from 80.6% to 119%. The method proves applicable for the quantification of NIIMs in environmental water, chicken meat and beef samples. Download: Download high-res image (196KB) Download: Download full-size image
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JOURNAL OF MOLECULAR STRUCTURE
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2025
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IF 4.7
Chuang Liu,Ying Li,Yu Zhang,Shiyu Li,Jun Dang
The discovery of tyrosinase modulators from natural products has long been hampered by limitations in screening efficiency and accuracy. In this study, a novel online screening system for tyrosinase was constructed based on HPLC technology that enables high-throughput recognition of active constituents in complex matrices. Applying this HPLC-tyrosinase system to Dracocephalum heterophyllum ( D. heterophyllum ), three active peaks were precisely captured, which were subsequently isolated and structurally characterized as caffeic acid, verbascoside, and rosmarinic acid. Enzyme activity assays revealed that caffeic acid (IC 50 = 1.08 mM) and rosmarinic acid (IC 50 = 0.41 mM) markedly inhibited tyrosinase activity, whereas verbascoside exhibited activating properties (EC 50 = 0.24 mM). The action mechanisms and bioactivities of these compounds were further elucidated through density functional theory calculations, molecular docking analysis, and in vivo validation. Collectively, the online HPLC-tyrosinase activity screening system established in this work not only provides a theoretical basis for the high value-added development of D. heterophyllum , but also delivers a high-throughput, precision tool for discovering natural tyrosinase inhibitors, demonstrating robust application potential in the fields of cosmetic science, food preservation and pharmaceutical development.
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MICROCHIMICA ACTA
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2025
·Vol. 192
·期 10
·1-12
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IF 5.3
Zhao Weiman,Fan Wenxiang,Liu Longchan,Gao Yingrui,Tong Ruonan,You Liying,Li Linnan,Wang Zhengtao,Yang Li
The precise and selective determination of ginsenosides, pharmacologically diverse saponins abundant in Panax species, is crucial for their therapeutic development and stringent quality control. However, inherent challenges, including their weak ultraviolet absorption and the high polarity imparted by sugar moieties, complicate their determination. Addressing these limitations, this study introduces the first-time construction and application of a boronate affinity dendritic mesoporous silica nanomaterial (BA-DMSN) as a highly efficient adsorbent for ginsenoside pretreatment. The synthesized BA-DMSN was comprehensively characterized, confirming a unique three-dimensional open dendritic framework, high specific surface area, and exceptional inner surface accessibility. These attributes facilitate rapid analyte adsorption and release, enabling a solid-phase extraction (SPE) process completed within approximately 10 min. Critically, the strategic incorporation of boronic acid groups conferred specific selectivity towards the cis-diol structures present in ginsenosides, allowing for their highly effective enrichment from complex matrices. Integrating this novel adsorbent with charged aerosol detection (CAD), a boronate affinity chromatography strategy was successfully developed and validated for the quantitative determination of nine key ginsenosides (notoginsenosides Fa, Fc, FP2, Fe, and ginsenosides Rc, Rd, Rb1, Rb2, Rb3) in stem-leaf extracts of Panax notoginseng. Methodological investigations demonstrated that this approach offers significant advantages over existing techniques, including operational simplicity, outstanding selectivity, and enhanced sensitivity, particularly for ginsenosides lacking strong chromophores. The successful analysis of actual Panax notoginseng samples underscores the robust applicability and promising prospects of the BA-DMSN-based SPE-CAD methodology for the quality control and further research of ginsenoside-based natural products. Graphical
研究领域:
分析化学
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纳米材料
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植物化学
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药物分析
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天然产物研究
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JOURNAL OF FOOD COMPOSITION AND ANALYSIS
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2026
·
IF 4.6
Zhihao Yang,Tianle Shen,Jinhu Tian,Yanbin Wang,Xingqian Ye,Jianchang Jin,Dan Wu
The determination of phenolic compounds serves as a critical approach for food quality control and screening of bioactive phytochemicals. This study developed a high-performance liquid chromatography-photodiode array detection (HPLC-PDA)-based analytical technique for plant phenolics, enabling simultaneous accurate quantification of 37 representative phenolic compounds in samples. Method validation demonstrated excellent linearity, precision, and accuracy, with intra-day and inter-day precision below 3 %, and spiked recoveries ranging from 96.88 % to 103.75 %. The methodology was successfully applied to analyze 19 distinct plant specimens, confirming its exceptional versatility. This method can be used as an efficient assay for plant polyphenols in multiple fields including food analysis, phytochemical research, and bioactive component development.
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MICROCHEMICAL JOURNAL
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2026
·
IF 5.1
Shiyu Li,Li Zhang,Haihua Zhang,Fang Yang,Jun Dang
Hyperlipidemia is closely linked to abnormal dietary lipid absorption, and pancreatic lipase (PL) is a key target for inhibiting intestinal lipid hydrolysis. Thus, the efficient discovery of PL inhibitors is crucial for treating the disease. However, existing recognition techniques suffer from false positives and disconnection from subsequent separation, hindering the exploration of natural product active components. This study developed an online high-performance liquid chromatography-fluorescence detection (HPLC-FLD) recognition system. It enables real-time mixing of chromatographic eluents with PL solution, forming protein-ligand complexes that yield characteristic negative peaks due to their lower fluorescence, thus enabling rapid localization of PL-binding components at corresponding retention times. Validation with orlistat as a reference standard confirmed the system's high precision, stability, and specificity. When applied to the crude extract of Sinacalia tangutica , this system recognized 15 active chromatographic peaks in a single analysis. Combined with an activity-guided progressive separation strategy, 16 compounds were obtained and exhibited PL inhibitory activity in vitro enzymatic assays. The therapeutic potential of phlorizin, one of inhibitors identified by our recognition system, was evaluated in hyperlipidemic mice. High-dose phlorizin lowered serum total cholesterol (TC) by 46.3% and triglyceride (TG) by 66.3%, reduced pancreatic PL content by 52.4%, raised fecal TG by 65.7%, alleviated hepatic steatosis and oxidative stress, with efficacy near orlistat. This integrated strategy of online recognition with activity-guided separation provides an efficient solution for the discovery of natural PL inhibitors with therapeutic potential.
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JOURNAL OF CHROMATOGRAPHY A
·
2026
·
IF 4
Zongkai Li,Xiaoqing Wang,Qianqian Wang,Zhi Li,Qiuhua Wu,Chun Wang
Endocrine-disrupting bisphenols as endocrine disrupting chemicals present significant risks to the human endocrine system. Developing accurate and highly sensitive methods for detecting trace levels of bisphenols in food is crucial to ensure food safety and prevent health risks. Herein, a hydroxyl-functionalized covalent organic framework (TD-COF) was synthesized using 4,4′,4′'-triaminotriphenylmethane and 3,3′-dihydroxy-[1,1′-biphenyl]-4,4′-dicarbaldehyde as monomer. TD-COF demonstrates superior adsorption ability for bisphenols compared with hydroxyl-free COF, which can be primarily attributed to the presence of hydrogen bonding and π-π interactions. By combining high performance liquid chromatography-mass spectrometry and solid phase extraction technology based on TD-COF, a method for analyzing four bisphenols in river water and chicken was established. Under optimal conditions, the method exhibits a low detection limit (river water: 0.03-0.15 ng mL -1 , chicken: 1.4-3.5 ng g -1 ), satisfactory spiked recovery (river water: 87.0-107%, chicken: 88.5-105 %) and good relative standard deviations (river water: 4.5-6.5%, chicken: 4.0-5.7%).
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高影响因子