JOURNAL OF CHROMATOGRAPHY A
·
2024
·
IF 3.8
Xue Li,Meng-Yao Wang,Yu Wang,Wen-Zhi Yang,Cheng-Xiong Yang
Efficient enrichment of trace zearalenone (ZEN) from the complex traditional Chinese medicine (TCM) samples is quite difficult, but of great significance for TCM quality control. Herein, we reported a novel magnetic solid phase extraction (MSPE) strategy for ZEN enrichment using the amino- and hydroxyl dual-functionalized magnetic microporous organic network (Fe 3 O 4 @MON-NH 2 -OH) as an advanced adsorbent combined with the high-performance liquid chromatography (HPLC) determination. Efficient extraction of ZEN was achieved via the possible hydrogen bonding, hydrophobic, and π-π interactions between Fe 3 O 4 @MON-NH 2 -OH and ZEN. The adsorption capacity of Fe 3 O 4 @MON-NH 2 -OH for ZEN was 215.0 mg g −1 at the room temperature, which was much higher than most of the reported adsorbents. Under the optimal condition, the developed Fe 3 O 4 @MON-NH 2 -OH-MSPE-HPLC method exhibited wide linear range (5–2500 μg L −1 ), low limits of detection (1.4–35 μg L −1 ), less adsorbent consumption (5 mg), and large enhancement factor (95) for ZEN. The proposed method was successfully applied to detect trace ZEN from 10 kinds of real TCM samples. Conclusively, this work demonstrates the Fe 3 O 4 @MON-NH 2 -OH can effectively extract trace ZEN from the complex TCM matrices, which may open up a new way for the application of MONs in the enrichment and extraction of trace contaminants or active constituents from the complex TCM samples.
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MICROCHEMICAL JOURNAL
·
2024
·
IF 4.9
Guanghou Wang,Xueqian Tang,Feixu Qin,Hongjin Wang,Hao Zhang,Hanyue Li,Lan Wei,Lixin Sun
Nauclea officinalis ( N. officinalis ), a medicinal plant of the genus Nauclea in the Rubiaceae family, is used to treat bronchitis, pneumonia and acute tonsillitis and enteritis in China. Extracts of N. officinalis include more than 60 alkaloids, which exert all kinds of pharmacological effects, such as antiproliferative, antiparasitic, antimicrobial, anticancer, and anti-inflammatory activities. In this study, an affinity ultrafiltration and high-performance liquid chromatography- tandem mass spectrometry (AUF-LC-MS/MS) approach was constructed and validated, and was applied to rapidly screen COX-2/5-LOX inhibitors in N. officinalis extracts (NOE). To gain a more comprehensive and profound understanding of the anti-inflammatory mechanism of N. officinalis . Central Composite Design (CCD) of Response Surface Method (RSM) was used to optimize extraction conditions for potential COX-2/5-LOX inhibitors from NOE. Next, COX-2/5-LOX dual targeted inhibitors were screened from NOE using AUF-LC-MS/MS, and the biological activity of the screened ligands was demonstrated by enzyme inhibition assay. Finally, the preferred binding modes for these COX-2/5-LOX inhibitors were then determined by molecular docking, and compared with active drugs celecoxib and zileuton, respectively, to further explore ligand active binding sites and intersections between ligands and target proteins. The optimum extraction conditions were follows: ethanol concentration of 79 %, liquid − solid ratio of 11.8 v / w and extraction time of 1.8 h. The results of COX-2 inhibition assay showed that angustine (AU) had the more stronger inhibition activity with an IC 50 of 20.49 μM, followed with IC 50 of angustidine (AD) and nauclefine (NF) were 35.89 and 60.45 μM, respectively. Among the three components, AU also exhibited the highest inhibition of 5-LOX with an IC 50 of 1.18 μM, followed by NF and AD at 2.75 and 4.35 μM, respectively. Owing to the synergistic effect of multiple components make NOE exhibit strong inhibitory activity, it is shown potent inhibitory activities with an IC 50 at 9.47 and 6.16 μg/mL for COX-2 and 5-LOX, respectively. This work has demonstrated that NF, AD, and AU are potential COX-2/5-LOX dual-target inhibitors, indicating that N. officinalis anti-inflammatory activities were partially based on these COX-2/5-LOX inhibitors. These research results can also be further used for developed or improved anti-inflammatory agents with more beneficial effects.
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FOOD CHEMISTRY
·
2025
·
IF 9.8
Huiyu He,Rui Wang,Rongbin Nie,Nan Dong
Pretreatment technology suffers from drawbacks such as tedious operation, low efficiency, and poor selectivity. Hence, we presented a singly capped cucurbit[7]uril-mediated magnetic solid phase extraction (Q[7]-MagSPE) combined with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) for multiresidue analysis of 20 pesticides. The Q[7]-MagSPE was constructed by assembling Q[7] onto the gold magnetic nanoparticles (GoldMag) via the reaction between one of the electron-rich carbonyl portals of Q[7] and gold. The host-guest interaction activity of supramolecules, the high dispersibility and easy separability of GoldMag were integrated in the Q[7]-MagSPE. The detection limits for 20 pesticides were lower than 10.3 ng/kg, and the recoveries were 71.55 – 110. 6 % . Moreover, the reusability of the Q[7]-GoldMag and effect of washing times on the pesticide residue were evaluated to be satisfactory. Therefore, the Q[7]-MagSPE provides a rapid and robust pretreatment method for the multiresidue determination of pesticides in vegetables, which is of great significance for food safety.
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Food Chemistry-X
·
2025
·
IF 8.2
Binbin Li,Qian Mu,Huijing Guo,Wenting Jia,Mengzhen Zhang,Ya Liu,Xinwen Jin
The effects of jujube pretreatment at different roasting temperatures (80–160 °C) on the dynamic changes in free amino acids and volatile organic compounds in jujube wine were evaluated using HPLC, HS-GC-IMS, HS-SPME-GC–MS, and sensory analysis. The results revealed that roasting at 80–100 °C enhanced the accumulation of sweet amino acids in jujube wine, whereas roasting at 140–160 °C increased the bitter amino acid content. As the roasting temperature increased, the contents of esters, alcohols, acids, aldehydes, and ketones in jujube wine rose initially before declining thereafter. Meanwhile, the furan compound content exhibited a continuous increase. Through multivariate statistical analyses, including orthogonal partial least squares-discriminant analysis (OPLS-DA), relative odor activity value (ROAV) calculations, and variable importance in projection (VIP), six key characteristic flavor compounds were identified. These included isoamyl acetate, ethyl hexanoate, and ethyl octanoate. The novel insights derived from this study could guide the improvement of jujube wine flavor.
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JOURNAL OF SEPARATION SCIENCE
·
2025
·Vol. 48
·期 2
·e70090
·
IF 2.8
Han Li,Xiaoming Wu,Yan Miao,Fengyu Dong,Xinjing Gui,Panpan Wang,Xuelin Li,Ruixin Liu
This study investigates the consistency of quality between the traditional decoction (TD) of Pheretima aspergillum and its dispensing granule decoction (DGD) by examining their chemical composition and antithrombotic efficacy. We first determined the nucleoside components, protein content, and volatile compounds in 10 batches of TD and 9 batches of DGD sourced from three manufacturers using high-performance liquid chromatography (HPLC), UV–vis spectrophotometry, and gas chromatography ion mobility spectrometry (GC-IMS). Next, we assessed antithrombotic efficacy by measuring the relative length of tail thrombosis and calculating the thrombus inhibition rates at 24 and 48 h. Our comprehensive analysis revealed that the concentrations of hypoxanthine, uridine, inosine, adenosine, and proteins in TD were significantly higher than those in DGD. Moreover, the types and concentrations of volatile compounds in TD and DGD exhibited substantial differences, with 19 volatile compounds identified as differentially present between the two decoctions. Despite these compositional differences, both decoction types demonstrated equivalent antithrombotic efficacy. Overall, the quality of DGD from manufacturers A and B aligned closely with that of TD. However, TD exhibited a higher overall quality compared to DGD, while both decoctions maintained consistent antithrombotic efficacy.
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JOURNAL OF CHROMATOGRAPHY A
·
2025
·
IF 4
Wen Hou,Ya-Qi Zhu,Yue-Jiao Yang,Qiong-Wei Yu
Loofah sponges (LS) were simply treated by alkaline solution and then used as solid-phase extraction (SPE) adsorbent to extract bisphenols from environmental water samples for the first time. As naturally material, LS exhibited an excellent adsorption performance for bisphenol compounds due to their particular functional groups such as hydroxyl, carboxyl, amino, and other active groups. Key extraction conditions were optimized, including adsorbent amount, washing solvent volume, sample pH, ionic strength, sample loading flow rate, eluent type, and elution solvent volume. Under the optimal extraction conditions (200 mg adsorbent amount and 5.0 mL eluent volume), a method was developed for analyzing five bisphenols in environmental waters by combining LS-based SPE with high-performance liquid chromatography-fluorescence detection (HPLC-FLD). This analytical method showed excellent linearity within BP concentration range of 0.5-500 ng/mL and low detection limits (0.077-0.225 ng/mL). The recoveries of five bisphenols ranged from 78.6 % to 112 % with inter-day and inter-day precision less than 5.1 %. This method was successfully applied to the analysis of bisphenols in water samples with various water sources including river, lake, tap water, bottled water, and barrelled water. The proposed analytical method is low-cost, efficient, and sensitive, offering an alternative strategy for monitoring bisphenols in enviromental water.
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2022
·
IF 3.318
Guiya Yang,Pai Liu,Huan Shi,Weixu Fan,Xie Feng,Jiabao Chen,Songsong Jing,Lei Wang,Yuguang Zheng,Dan Zhang,Long Guo
The rhizome of Dioscorea nipponica Makino (RDN) is a widely used herbal medicine, which has significant anti-inflammatory activities on various inflammatory diseases. However, the bioactive compositions responsible for the anti-inflammatory activity of RDN are still unknown. This study aimed to identify the anti-inflammatory bioactive compounds in RDN using high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (HPLC-Q/TOF-MS), quantitative analysis of multiple components by single marker (QAMS) and chemometric methods. Firstly, an HPLC-Q/TOF-MS method was employed for identification of bioactive steroidal saponins in RND, and a total of twelve steroid saponins were identified. Then, QAMS method was employed to determine the contents of seven bioactive steroidal saponins, including protodioscin, protogracillin, methyl protodioscin, pseudoprotodioscin, pseudoprogracillin, dioscin and gracillin in RND samples using dioscin as the reference analyte. The anti-inflammatory effects of RDN samples were then evaluated by inhibition of NO production in LPS-induced RAW264.7 cells. Furthermore, chemometric methods, including Pearson correlation analysis and partial least squares regression (PLSR) were employed to investigate the correlations between chemical components and anti-inflammatory activities, and explore the potential anti-inflammatory bioactive compounds of RDN. The results indicated that protodioscin, dioscin and gracillin were selected as the major anti-inflammatory compounds in RND. The further verification experiments showed that protodioscin, dioscin and gracillin exhibited great inhibition on NO production with IC 50 values (the half maximal inhibitory concentration) of 0.712 μM, 0.469 μM and 0.815 μM, respectively. They also significantly reduced the levels of TNF-α, IL-1β, and IL-6 in LPS-induced RAW264.7 cells. The present study provided evidences for the anti-inflammatory activity of RND and identification of the anti-inflammatory components in RDN.
研究领域:
生药学
·
药物分析
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药理学
·
分析化学
·
生物化学
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MICROCHEMICAL JOURNAL
·
2020
·
IF 3.594
Xu Jing,Jiaohui He,Wenfei Zhao,Xin Huang,Xiaowen Wang
High-performance liquid chromatography (HPLC) determination of phenolic endocrine disrupting chemicals in bottled beverages was carried out using effervescent tablet-assisted switchable hydrophilicity solvent-based microextraction with solidification of floating organic droplets (ETA-SHS-ME-SFO). Octanoic acid was used as the extractant, which is a hydrophobic form of a switchable hydrophilicity solvent. The extractant was generated in-situ by the reaction between sodium octanoate and citric acid and collected after solidification in an ice-bath. Carbon dioxide gas was produced by the reaction between sodium bicarbonate and citric acid, which assisted the extraction of target compounds. Good linearity was obtained over the range of 0.03–3 µg mL −1 , with a correlation coefficient greater than 0.998. The relative recovery varied from 71.7% to 98.1%. The limit of detection ranged from 0.0002 to 0.0007 µg mL −1 . The intra- and inter-day relative standard deviations ( n = 3) were less than 5.8%. Finally, the proposed method was successfully applied to the determination of the levels of bisphenol A, 4-nonylphenol, and 4-tert-octylphenol in bottled water, juice, and energy drink.
研究领域:
分析化学
·
环境科学
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Environmental Sciences Europe
·
2019
·Vol. 31
·期 1
·1-10
·
IF 5.878
Zhou Qingxiang,Wu Yalin,Yuan Yongyong,Zhou Xianqi,Wang Hongyuan,Tong Yayan,Zhan Yali,Sun Yi,Sheng Xueying
Background Sudan red dyes are widely used as color additions in various fields. Due to their potential carcinogenicity and large consumption, they have absorbed much more attention and become a research hot topic. There have been a few of existing methods for their analysis from samples; however, it is of great importance to develop simple, sensitive, and low-cost analytical method for public health and safety. This article described a new method based on magnetic Fe@NiAl-layered double hydroxides for enrichment of Sudan red dyes in combination with high-performance liquid chromatography. Results The as-prepared magnetic Fe@NiAl-layered double hydroxides (Fe@NiAl-LDHs) exhibited good adsorption capacity for Sudan red dyes, and could be used as an effective adsorbent for preconcentration of three Sudan Red dyes from environmental water samples. The proposed method provided low limits of detection in the range of 0.002–0.005 μg L −1 with magnetic solid-phase extraction in combination with high-performance liquid chromatography. Conclusion The developed method utilized the easy to prepare magnetic materials as adsorbents and conventional analytical instrument and provided high sensitivity, which provided a robust and low consumption of toxic organic solvent alternative method. The results of present study are of great value for interested laboratories to monitor the level of Sudan red dyes in water samples or develop sensitive determination methods to monitor other pollutants at trace level in environmental waters.
研究领域:
分析化学
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环境科学
·
食品安全
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Food Analytical Methods
·
2017
·Vol. 10
·期 12
·3847-3855
·
IF 2.038
Sun Bin,Wang Chunpeng,Wang Qi,Chen Ling,Dang Xueping,Huang Jianlin,Chen Huaixia
An acryloyl β -cyclodextrin (A- β -CD) monolithic column for solid-phase microextraction (SPME) and determination of carbofuran and carbaryl by high-performance liquid chromatography (HPLC) have been prepared through a “one-step” polymerization method. The synthesis conditions, including the volume of cross-linker, the ratio and volume of mixed porogenic solvent consisted of methanol and N,N -dimethylformamide were optimized. The prepared monolithic column was characterized by thermogravimeteric analysis (TGA), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), and Brunner-Emmet-Teller (BET) measurement. The eluent type, volume and flow rate, sample volume, flow rate, acidity, and ionic strength were optimized in detail. Under the optimized conditions, a simple, rapid, and sensitive SPME-HPLC method was developed for determination of carbofuran and carbaryl in rice samples. The method yielded a linear calibration curve in the concentration ranges of 1.5–200 μg/kg for carbofuran and 0.3–200 μg/kg for carbaryl with correlation coefficients ( R
2 ) of above 0.9955. Limits of detection ( S / N = 3) were 0.5 μg/kg for carbofuran and 0.1 μg/kg for carbaryl, respectively. The recoveries of this method ranged from 88.1 to 105.8%. The relative standard deviations were less than 8.1%.
研究领域:
分析化学
·
食品科学
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NUCLEAR MEDICINE AND BIOLOGY
·
2026
·
IF 3.1
Lei Xu,Zhenhao Dong,Hong Zhang,Antonio Arleques Gomes,Wagner de Rossi,Jing Wang,Arian Pérez Nario,Qinggang He
A post-column derivatization high-performance liquid chromatography-ultraviolet (HPLC-UV) method was developed to determine Kryptofix 2.2.2 (K2.2.2) in PET tracers. This method utilizes the specific complexation between K2.2.2 and Pb 2+ , forming a stable 1:1 host-guest complex. The complexation produces a bathochromic shift in UV absorption maximum (from 210 nm to 254 nm), enabling sensitive detection. This approach addresses the limitations of poor performance and narrow applicability associated with direct single-method detection of K2.2.2. The chromatographic conditions were optimized (column flow rate: 0.7 mL·min −1 ; derivatization reagent flow rate: 0.7 mL·min −1 ; Pb 2+ concentration: 50 μg·mL −1 ) and the method was validated. The results exhibited excellent linearity (1–100 μg·mL −1 , r 2 > 0.999), high reproducibility (relative standard deviation (RSD) < 5%), and a low detection limit (0.5 μg·mL −1 ). The method successfully quantified K2.2.2 in [ 18 F]FDG, [ 18 F]AV45 and [ 18 F]DPA714, achieving spiked recoveries of 89%–105%. Additionally, the method remained unaffected by interference from common sample components such as sodium chloride and sodium ascorbate. This method provides a novel and efficient quality control tool for the simultaneous analysis of radiochemical purity and K2.2.2 content in diverse PET tracers.
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Frontiers in Plant Science
·
2024
·
IF 4.1
Li Shuang,Yang Lei,Wang Min,Chen Yang,Yu Jianjun,Chen Hao,Yang Haijian,Wang Wu,Cai Zhiyong,Hong Lin
Introduction: Citrus fruit is rich in important functional constituents such as flavonoids, phenolic acids terpenes and other functional substances that play an important role for treating clinical diseases or controlling major agricultural diseases and pests. Plant secondary metabolites have become one of the most important resources of novel lead compounds, especially young citrus fruits contain multiple functional substances. ‘Orah’, a type of citrus reticulata, is known for its fine appearance, productivity, delicious sweetness, late-maturing characteristics, and is widely cultivated in China. Fruit thinning and rootstock selection are commonly used agronomic measures in its production to ensure its quality and tree vigor. However, few studies have demonstrated the effects of these agronomic measures on the functional substances of ‘Orah’.Methods: In this study, we used HPLC coupled with UV to detect the dynamic changes of fruit quality, 13 main flavonoids, 7 phenolic acids, 2 terpenes, synephrine and antioxidant capacity in both peel and pulp of citrus fruits grafted on four rootstocks (Red orange Citrus reticulata Blanco cv. red tangerine, Ziyang xiangcheng Citrus junos Sieb. ex Tanaka, Trifoliate orange Poncirus trifoliata L. Raf, and Carrizo citrange Citrus sinensis Osb.×P.trifoliate Raf) at six different developmental stages (from 90 DAF to 240 DAF).Results: The results indicated that rootstock can significantly affect the contents of functional constituents and antioxidant capacity in ‘Orah’. Additionally, it was found that pruning at either 90 DAF (days after flowering) or 150 DAF produced the most favorable outcomes for extracting functional substances. We also identified rootstock ‘Trifoliate orange’ has the highest total soluble solids (TSS) and ‘Ziyang xiangcheng’ to be the optimal in terms of comprehensive sensory of fruit quality, while ‘Red orange’ and ‘Ziyang xiangcheng’ are optimal in terms of functional substance quality, and ‘Red orange’ excels in antioxidant capacity.Discussion: Overall, the findings demonstrate the important role of rootstocks and developmental stage in shaping fruit sensory quality and functional substance synthesis, providing valuable insights for guiding rootstock selection, determining thinning time, and utilizing pruned fruits in a more informed manner.
研究领域:
农业
·
植物科学
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食品科学
·
药理学
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危险品化学品经营许可证（带存储）