MOLECULES
·
2026
·Vol. 31
·期 12
·2138
·
IF 5.1
Xiaoduo Ma,Lei Xing,Ranran Feng,Shumin Hu,Wei Yong,Tianyang Guo,Zhaoxia Yang,Huanlu Song
Whisky is well-known worldwide owing to its unique flavor, and its fermentation and distillation conditions have a significant effect on its aroma. In this paper, new-make spirits were prepared by four fermentation conditions (two distilling yeasts and two fermentation temperatures), and the different stages (wort, wash, low wine, and new-make spirit) of the samples were collected. The main aroma compounds and their precursors were initially determined in wort and wash samples by GC-MS, UPLC-MS and HPLC. Results showed that Strecker degradation, reduction, and esterification occurred during the fermentation process, leading to decreased contents of amino acids and increased contents of volatile esters, alcohols, and acids. Moreover, the two distilling yeasts exhibited their respective optimal fermentation temperatures. Then, the distillation process was evaluated by two-dimensional gas chromatography–olfactory–mass spectrometry (GC×GC-O-MS), and 74 aroma compounds were found in different stages of new-make whiskies fermented by the two distilling yeasts and one brewer’s yeast. The contents of most compounds were enhanced by at least ten times after two distillations, while the contents of some sulfur compounds decreased. Finally, the feature aroma-active compounds of each new-make whisky were identified according to rOAV. These results provided theoretical and methodological support for yeast selection and process control in whisky production.
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高影响因子
MOLECULES
·
2022
·Vol. 28
·期 1
·295
·
IF 4.927
Mengyu Li,Hui Luo,Zhen Huang,Jin Qi,Boyang Yu
Erdong Gao (EDG), consisting equally of roots of Asparagi Radix and Ophiopogonis Radix, is a well-known traditional Chinese formulation that has been used to treat cough and throat pain for centuries. However, the bioactive components in EDG remain to be elucidated. In this study, a rapid and effective method involving live cell bio-specific extraction and HPLC-Q-TOF-MS/MS was established to rapidly screen and identify the anti-inflammatory compounds of an EDG extract. One hundred and twenty-four components were identified in EDG extract using HPLC-Q-TOF-MS/MS analysis. After co-incubation with 16HBE, HPAEpiCs and HUVECs, which have been validated as the key target cells for pulmonary diseases, sixteen components were demonstrated to exhibit an affinity for binding to them. Furthermore, fifteen components were subsequently verified to exert anti-inflammatory effects on lipopolysaccharide (LPS)-induced 16HBE, HPAEpiCs and HUVECs via inhibiting the release of TNF-α and IL-6, indicating that nine steroidal saponins may possess potential for the treatment of lung-related diseases. Taken together, our study provides evidence that live cell biospecific extraction combined with the HPLC-Q-TOF-MS/MS technique was an efficient method for rapid screening potential bioactive components in traditional Chinese medicines and the structure activity relationship of steroidal saponins in EDG was summarized for the first time.Keywords:Erdong Gao;anti-inflammatory;steroidal saponins;structure activity relationship;cell extraction
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高影响因子
MICROCHEMICAL JOURNAL
·
2023
·
IF 4.8
Yachao Hao,Wei Zhou,Xin Wang,Youping Liu,Xin Di
In this study, a magnetic graphene oxide modified with green carboxyl-based deep eutectic solvent (MGO@DES) was synthesized for the first time and employed as a highly efficient adsorbent for the magnetic solid-phase extraction (MSPE) of three estrogens in milk samples. With large specific surface, good hydrophobicity and abundant adsorption sites, MGO@DES exhibited excellent extraction performance for estrogens. The adsorption kinetic experiment revealed that 5 mg of MGO@DES reached the equilibrium of estrogen adsorption within 3 min. MGO@DES based MSPE coupled with HPLC-UV method was developed and applied to the determination of three estrogens in milk samples. Good linearity (R 2 > 0.9953) was obtained in the range of 1–200 ng mL −1 and the low limits of detection were 0.20–0.28 ng mL −1 . The spiked recoveries were in the range of 90.3–105.7%, with RSDs less than 7.9%.
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JOURNAL OF SEPARATION SCIENCE
·
2021
·Vol. 44
·期 11
·2269-2278
·
IF 3.645
Xuelei Chen,Wei Li,Jingguang Li,Sai Fan,Zhixiong Shi
Organophosphorus flame retardants are a class of widely used plasticizers and flame retardants. In this study, an analytical methodology for the simultaneous determination of 13 organophosphorus flame retardants in milk was developed by using high-performance liquid chromatography-tandem mass spectrometry in combination with a modified quick, easy, cheap, effective, rugged, and safe technique and solid-phase extraction. The experimental parameters of the sample purification procedure and high-performance liquid chromatography-tandem mass spectrometry were optimized. The developed method was validated in terms of linearity, limits of detection, recovery, and precision. The method showed a linear response in the 1–100 ng/mL concentration range and the limits of detection ranged from 0.001 to 0.3 ng/mL. The mean recoveries for most organophosphorus flame retardants were in the ranges of 75.0–115.8% (spiked at 2.5 ng/mL) and 76.7–124.8% (spiked at 25 ng/mL), with relative standard deviations of <13.09%. The developed methodology was successfully applied to the analysis of nine human milk samples and nine commercial cow milk samples. Eleven organophosphorus flame retardants were detected in the human milk samples, with median concentrations that ranged from lower than the limit of detection to 1.47 ng/mL, and only nine organophosphorus flame retardants were detected in cow milk samples, with median levels of <0.32 ng/mL.
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Drug Design Development and Therapy
·
2020
·
IF 3.216
Hao-Zhen Zheng,Xiao Shen,Ying-Ying He,Xiang-Li Yan,Sheng-Xin Wang,Ai-Ming Yu,Li-Sheng Wang
Objective The aim of our research was to analyze and compare the pharmacokinetics of paeoniflorin, calycosin, calycosin-7-o-β-d-6-glucoside, and 6-gingerol in the blood and brain tissue of normal and cerebral ischemia-reperfusion injury rats by HPLC-MS/MS method.Methods The blood and brain tissue samples of normal and middle cerebral artery occlusion (MCAO) rats were compared. The blood and brain tissue samples were collected by using microdialysis technique. The concentrations of paeoniflorin, calycosin, calycosin-7-o-β-d-6-glucoside, and 6-gingerol in blood and brain tissues were determined by the HPLC-MS/MS internal standard method.Results Compared with the normal group, the model group after the administration of the Huangqi Guizhi Wuwu Decoction showed that Cmax blood, AUC0-t blood, and AUC0-inf blood of paeoniflorin were increased, CLblood, t1/2 brain, and Vbrain of paeoniflorin were decreased; Cmaxblood, AUC0-tblood, AUC0-infblood, and average residence time (MRTbrain) of calycosin-7-o-β-d-6-glucoside were decreased and the CLblood and Cmax brain of calycosin-7-o-β-d-6-glucoside were increased; Cmax blood of calycosin was decreased, Vblood and Vbrain of calycosin were increased; Cmax blood, AUC0-t blood, AUC0-inf blood, and MRTbrain of 6-gingerol were decreased, CLblood of 6-gingerol was increased.Conclusion This method is simple, rapid, and sensitive. It is suitable for the pharmacokinetic study of Huangqi Guizhi Wuwu Decoction in the blood and brain tissue of rats. Cerebral ischemia-reperfusion injury increased the content of paeoniflorin, calycosin, calycosin-7-o-β-d-6-glucoside, and 6-gingerol in the blood, affecting the clearance rate of paeoniflorin in the brain, the detention time of calycosin-7-o-β-d-6-glucoside and the 6-gingerol in the brain. In normal and cerebral ischemia-reperfusion rats, the content of paeoniflorin and 6-gingerol in the blood was higher than that in brain tissue, while the content of calycosin, calycosin-7-o-β-d-6-glucoside in the brain tissue was higher than that in blood, suggesting that calycosin and calycosin-7-o-β-d-6-glucoside have brain targeting properties.
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高影响因子
CLINICA CHIMICA ACTA
·
2018
·
IF 2.926
Feiyan Liu,Luyang Xu,Changcheng Sheng,Xiaoyan Qiu,Ming Zhang,Zheng Jiao
Background The immunosuppressive agent mycophenolic acid (MPA) is a non-competitive, reversible inhibitor of inosine-5′-monophosphate dehydrogenase (IMPDH). Thus, IMPDH activity can serve as a potential pharmacodynamic biomarker to optimize dosing of MPA. Methods Peripheral blood mononuclear cells were isolated from 2 mL blood samples and an in vitro enzymatic reaction was subsequently performed for 120 min. To determine IMPDH activity in Chinese healthy volunteers and renal transplant patients, a high performance liquid chromatography assay was established and validated by subtracting adenosine monophosphate (AMP) from blank samples for eliminating exogenous AMP interference. Results The accuracy of our method ranged between −0.8% and 12.5%, and the precision ranged between 0.7% and 6.3%. The mean value of IMPDH activity across 11 healthy volunteers was 46.60 ± 14.28 μmol/s/mol AMP. A negative relationship between MPA concentration and IMPDH activity was observed in four renal transplant patients treated with MPA 13 days post-transplantation, while the inhibitory rate of IMPDH activity ranged from 24% to 42%. Conclusion A bioanalytical assay for IMPDH quantification was optimized and evaluated. The differences in the pharmacodynamics of MPA between Asians and Caucasians may provide some evidence for dosing differences among ethnicities.
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高影响因子
CHROMATOGRAPHIA
·
2018
·Vol. 82
·期 8
·1285-1293
·
IF 1.401
Wang Huimin,Guo Bin,Pang Xiaoya,Yu Huan,Liu Haiyan,Yan Hongyuan,Han Dandan,Guo Huaizhong,Bai Ligai
A poly(NMA-ST- co -TAIC-EDMA) monolithic column was prepared by redox initiation method using N -methylolacrylamide (NMA) and styrene (ST) as co-monomers. The composite monolith was characterized by scanning electron microscopy (SEM) and nitrogen adsorption–desorption isotherm and was used as a solid phase extraction (SPE) absorbent for enrichment of β -sitosterol by high performance liquid chromatography (HPLC). Under the optimum conditions for extraction and determination, the calibration equation was y = 1.02247 x + 0.1766; the linear range was 0.015–0.75 mg mL −1 and the linear regression coefficient was 0.998. The limit of detection (LOD) and the limit of quantification (LOQ) were 0.006 mg mL −1 and 0.02 mg mL −1 , respectively. The spiked recoveries of β -sitosterol in edible oil samples were 83.60–103.88%; precisions for intra-day and inter-day assays presented as relative standard deviations were less than 6.0% and 6.2%, respectively. The enrichment factor of β -sitosterol was 60 and the results showed that the monolithic column had high selectivity and good permeability as an on-line SPE absorbent for the enrichment and determination of β -sitosterol from edible oils.
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高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2018
·Vol. 41
·期 18
·3508-3514
·
IF 2.415
Ling Chen,Xueping Dang,Youhong Ai,Huaixia Chen
An acryloyl β-cyclodextrin-silica hybrid monolithic column for pipette tip solid-phase extraction and high-performance liquid chromatography determination of methyl parathion and fenthion has been prepared through a sol–gel polymerization method. The synthesis conditions, including the volume of cross-linker and the ratio of inorganic solution to organic solution, were optimized. The prepared monolithic column was characterized by thermogravimetric analysis, scanning electron microscopy, and Fourier transform infrared spectroscopy. 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 and sensitive pipette tip solid-phase extraction with high-performance liquid chromatography method was developed for the determination of methyl parathion and fenthion in lettuce. The method yielded a linear calibration curve in the concentration ranges of 15–400 μg/kg for methyl parathion and 20–400 μg/kg for fenthion with correlation coefficients of above 0.9957. The limits of detection were 4.5 μg/kg for methyl parathion and 6.0 μg/kg for fenthion, respectively. The recoveries of methyl parathion and fenthion spiked in lettuce ranged from 96.0 to 104.2% with relative standard deviations less than 8.4%.
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TALANTA
·
2018
·
IF 4.244
Quan Wang,Shigang Shen
A novel porous monolithic column was synthesized via in situ free-radical polymerization within a stainless steel column (50 × 4.6 mm i.d.) by using triallyl isocyanurate and methyl methacrylate as co-monomers, ethylene glycol dimethacrylate as a crosslinking agent, 1,4-butanediol, 1- dodecanol , and N, N-dimethylformamide as tri-porogens, and azobisisobutyronitrile as an initiator. The optimized monolithic columns were investigated by scanning electron microscopy, a nitrogen absorption-desorption apparatus, and mercury intrusion porosimetry. The effect of mobile phase composition and temperature on chromatographic behavior was studied in detail as well. The results showed that homemade monolithic columns not only have relative uniform porosity structure, low back pressure, and high thermal stability, but also show high column efficiency, the theoretical plates number of the new polymer monolithic column exceeded 31,000 plates m −1 . Good resolution was achieved for HPLC separation of small molecules, including polycyclic aromatic hydrocarbons , isomers of phenols, and the Chinese herbal medicine notoginseng. Methodological validation of six drugs in notoginseng show that correlation coefficients of the linear regressions were in the range of 0.9989–0.9997; the value of relative standard deviation for precision were in the range of 1.37–4.21% for intra-day and 0.34–5.31% for inter-day, respectively; the values of accuracy expressed by recovery were in the range of 100.57–102.51%, 95.18–102.68%, 101.61–102.82%, 100.94–102.40%, 100.99–103.15% and 99.49–103.91% for the six drugs in order, respectively. Taking aromatic hydrocarbons as samples, the relative standard deviation values of the run-to-run (n = 5) and column-to-column (n = 5) based on peak area were < 2.01% and 2.39%, and two RSDs based on retention time were < 2.56% and 2.23%, respectively. The result showed that the polymer monolithic column has good separation ability and high permeability for small molecular substances.
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MICROCHIMICA ACTA
·
2017
·Vol. 184
·期 8
·2715-2721
·
IF 4.58
Wang Chenlu,Zhou Wei,Liao Xiaoyan,Zhang Wenpeng,Chen Zilin
Polyether ether ketone (PEEK) is an ideal substrate for in tube solid-phase microextraction (SPME) because it overcomes the shortcomings of conventional silica fibers in terms of fragility and poor flexibility. Commonly used bare PEEK tubes suffer from difficult modification with selective sorbents and low inner surface areas. This problem was solved by etching with concentrated sulfuric acid, which dissolves the amorphous regions of the PEEK surface and yields a rough inner surface with plenty of microscopically small holes. The etched tube was then stepwise functionalized with polydopamine and graphene oxide which was in-situ immobilized. The modified tube displays excellent efficiency for the extraction of positively charged quaternary alkaloids by a mixed-mode extraction. Enrichment factors from 221 to 275 can be obtained for the extraction of the alkaloids jatrorrhizine, palmatine and berberine. The alkaloiods were then quantified by online SPME-HPLC-MS/MS detection. The method has detection limits of 0.1 pg mL −1 , good linearity, and good intra-day reproducibility (≤ 2.4%). It was applied to the analysis of the three alkaloids in Cortex Phellodendri herb and rat plasma after oral administration.
A concentrated sulfuric acid etching method was used for enhance the workability of polyether ether ketone tube (PEEK) in solid phase microextraction (SPME). The etched tube was covered with graphene oxide (GO) for extraction of protoberberines.
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JOURNAL OF CHROMATOGRAPHY A
·
2024
·
IF 3.8
Jiaming Yuan,Jincai Wang,Zhixu Chen,Yuexiang Chang,Litong Chen,Zhizeng Gao,Jacques Crommen,Tingting Zhang,Zhengjin Jiang
In this study, a novel at-line nanofractionation platform was established for screening SARS-CoV-2 fusion inhibitors from natural products for the first time by combining HPLC-MS/MS with high-throughput fluorescence polarization (FP) bioassay. A time-course FP bioassay in 384 well-plates was conducted in parallel with MS/MS to simultaneously obtain chemical and biological information of potential fusion inhibitors in Lonicerae Japonicae Flos (LJF) and Lianhua Qingwen capsules (LHQW). Semi-preparative liquid chromatography and orthogonal HPLC separation were employed to enrich and better identify the co-eluted components. After comprehensive evaluation and validation, 28 potential SARS-CoV-2 fusion inhibitors were screened out and identified. Several compounds at low micromolar activity were validated by in vitro inhibitory assay, molecular docking, cytotoxicity test, and pseudovirus assay. Moreover, four potential dual-target inhibitors against influenza and COVID-19 were discovered from LJF using this method, offering novel insights for the development of future pharmaceuticals targeting epidemic respiratory diseases.
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MICROCHEMICAL JOURNAL
·
2025
·
IF 5.1
Peiyi Jin,Liping Wang,Linzhou Chen,Jinjian Zhong,Tiefeng Yuan,Jiaju Pi,Jilong Huang,Lin Gan,Huajun Fan
To obtaining diosgenin from Dioscorea nipponica Makino ( D. nipponica ) was usually subjected to the multiple processes such as extraction, hydrolysis, transformation and separation etc. In this study, a novel method for rapid production and recovery of diosgenin from D. nipponica was developed by integrating microwave-assisted extraction (MAE), microwave-assisted hydrolysis (MAH) and two-phase extraction (TPE) in one-step procedure, that named MAEH-TPE. Using a two-phase system of ethanol aqueous solution-sulfuric acid-petroleum ether, the MAEH-TPE process was optimized by single-factor experiments and response surface methodology (RSM). Under optimum conditions of ethanol aqueous solution of 60 % (v/v), sulfuric acid concentration of 1.4 mol/L, liquid-to-material ratio of 20 mL/g, extraction temperature of 90 ℃, and extraction time of 35 min, the yield of diosgenin reached 17.09 ± 0.32 mg/g which conformed very closely to the predicted value of 17.185 mg/g, and validation experiments confirmed effectiveness and reliability of the RSM model. Compared with the conventional methods, MAEH-TPE exhibited higher extraction yield, shorter extraction time and simpler operation. The mechanism in MAEH-TPE process was explored in detail by chromatographic analysis and multi-phase equilibria. Enzyme inhibition assay demonstrated that the inhibition rate of the extracted diosgenin on porcine pancreatic lipase (PPL) reached 56.18 ± 1.38 % with IC 50 of 191.42 µg/mL, further proving that diosgenin as the main parent structure of the saponins in D. nipponica dominantly contributed to PPL inhibitory effect. Also, the results proved that MAEH-TPE had excellent extraction performance and simplified the complex processes, reducing energy consumption and saving solvents and resources.
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危险品化学品经营许可证（带存储）