ANALYTICAL AND BIOANALYTICAL CHEMISTRY
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2026
·
IF 4.1
Zhou Xinyue,Duan Sufei,Lou Yuye,Deng Yue,Feng Shuang,Liu Jiale,Zhang Jiarui,Xi Yalin,Shi Meiyun,Yin Lei
A sensitive UPLC-MS/MS method was developed and validated for quantifying polyethylene glycol 1000 (PEG1000) in zebrafish tissues, featuring a systematic comparison of two MS acquisition strategies. Through comprehensive optimization, the ammonium adduct [M+NH 4 ] + of the representative 18-EO oligomer ( m/z 828.5) was selected as the precursor ion, achieving approximately fourfold higher signal intensity than [M+H] + . Critically, the conventional high declustering potential in-source CID approach monitoring fragment ions was outperformed by the optimized MRM method monitoring the intact ammoniated precursor, which demonstrated 2.7-fold signal enhancement and superior selectivity. The integration of micro-solid-phase extraction (μ-SPE) further improved method performance, yielding 1.5-fold signal gain and markedly reduced matrix effects compared to conventional protein precipitation. The fully validated method exhibited excellent linearity (0.5–50 μg/mL, r > 0.995), accuracy, precision, and stability. Application to zebrafish tissue distribution studies revealed pronounced organ-specific accumulation following aqueous exposure to 200 μg/mL PEG1000, with highest concentrations in intestine tissue exhibiting a time-dependent increase, followed by muscle, while muscle maintained consistently low levels. This analytical platform, synergistically combining μ-SPE cleanup and ammoniated adduct-based MRM, offers superior sensitivity over in-source CID approaches and provides a practical framework for polymer bioanalysis, yielding critical insights into the in vivo fate of PEG-based compounds. The key novelties of this work are the following: (i) the first systematic comparison between ammoniated adduct MRM and high-DP in-source CID for PEG1000 quantification; (ii) the introduction of μ-SPE for sample preparation in zebrafish tissues, achieving 1.5-fold signal enhancement; and (iii) the successful application of this platform to reveal organ-specific accumulation patterns of PEG1000. Graphical abstract
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高影响因子
FOOD RESEARCH INTERNATIONAL
·
2026
·
IF 8
Xiaomin Cao,Hanna Cai,Hongyan Zhang,Xianghao Yuan,Siyi Pan
Medicinal and edible citrus resources are widely utilized in traditional Chinese medicine and daily diets due to their abundant health-promoting properties. However, systematic comparative studies on their sensory characteristics, phytochemical profiles, and biological activities remain insufficient, particularly among different varieties. In this study, electronic tongue analysis, UPLC-Q-TOF-MS/MS, spectrophotometry, and molecular docking were employed to evaluate the sensory attributes, chemical composition, and antioxidant activity of five medicinal and edible citrus resources. Electronic tongue analysis indicated that the Citri sarcodactylis fruct (CSF) exhibits the strongest sourness and bitterness. Citri exocarpium rubrum (CER), Citri grandis exocarpium (CGE), and Guangchenpi (GCP) exhibited strong antioxidant activity, while CSF showed the lowest activity. The ethanol precipitation supernatant (HTAPS) fraction exhibited significantly stronger antioxidant activity than the ethanol precipitation (HTAP). Furthermore, a total of 75 compounds were tentatively identified from five citrus resources, and multivariate analysis revealed key differential metabolites, including polymethoxyflavones, flavanones, and limonoids. Limonin, naringin, hesperidin, hesperetin, apiin, and isosinensetin exhibited strong binding affinity with Keap1 (PDB ID: 4IQK ) protein. This study provides a multidimensional basis for the high-value utilization of medicinal and edible citrus resources in functional foods and health products.
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FOOD CHEMISTRY
·
2026
·
IF 10.4
Mengyang Hou,Yujuan Zhou,Ka Wing Cheng,Rongrong Luo,Chengyuan Lin,Lin Zhu,Zhaoxiang Bian
This study first established a green, integrated process coupling ultrasound-assisted natural deep eutectic solvent (UA-NADES) extraction with macroporous resin purification to obtain Chinese quince total phenolics (CQ-TP). L-proline/glycerol (molar ratio 2:5; Pro-Gly) was identified as the optimal extraction solvent among eleven synthesised NADESs and four common solvents. The optimised UA-NADES extraction process (35% water in Pro-Gly, 40 °C, 300 W, 36 min, liquid-to-solid ratio 30 mL/g) yielded 59.14 ± 0.65 mg/g CQ-TP, markedly higher than the yields from conventional methods. NKA-9 resin showed superior adsorption and desorption performance for CQ-TP, with adsorption behavior consistent with the Langmuir isotherm and a pseudo-second-order kinetic model. Column purification achieved a CQ-TP purity of 72.54 ± 0.81%. Finally, nine main phenolic constituents in the purified CQ-TP extract were quantified by UPLC–TQ–MS/MS to enable batch-to-batch consistency monitoring. This work will significantly contribute to the valorization of Chinese quince phenolics and the development of natural antioxidants.
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2023
·
IF 3.4
Xuelong Zhao,Ruixue Dai,Jing Wang,Liangliang Cao,Peidong Chen,Weifeng Yao,Fangfang Cheng,Beihua Bao,Li Zhang
Cayratia japonica ointment has been used for many years to promote wound healing after perianal abscess surgery. This study aimed to determine the skin-permeable and skin-retainable components of Cayratia japonica ointment after topical application to intact or broken skin via UPLC-Q-TOF-MS/MS analysis and in vitro transdermal assay . Moreover, a combination of semi-quantitative and molecular docking analyses was performed to identify the main active components of the Cayratia japonica ointment and the probable phases of the wound healing process that they act on. Modified vertical Franz diffusion cells and abdominal skin of rats were selected for the in vitro transdermal study. Mass spectrometry data were collected in both positive and negative ion modes. A total of 7 flavonoids (schaftoside, luteolin-7-O-glucuronide, luteolin-7-O-glucoside, apigenin-7-O-glucuronide, luteolin, apigenin, and chrysin) and 1 coumarin (esculetin), were found to permeate and/or retained by intact or broken skin. Among them, the flavonoids were more permeable through intact/broken skin and exhibited stronger binding affinities for targets related to the inflammatory and proliferative phases of wound healing. This study suggests that the flavonoids in Cayratia japonica ointment are most likely the main active components and are crucial at the inflammatory and proliferative phases of wound healing.
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2023
·
IF 3.4
Yao Wang,Yuhan Liu,Yutong Sha,Jia Li,Luyao Han,Huili Chen,Shengdi Su,Ning Li,Xijing Chen,Di Zhao
A chiral UPLC-MS/MS method was developed and validated to determine oxiracetam enantiomers in human plasma, urine, and feces. The R-Oxiracetam and S-Oxiracetam were quantified using a CHIRALPAK ®AD3 column at 25 ℃, and the resolution was greater than 3.2. The S-Oxiracetam is the eutome r that isresponsible for the treatment of various brain damage. Isocratic elution was conducted at a flow rate of 0.9 mL/min for 6 min using the mixture of methanol and acetonitrile (methanol:acetonitrile, 15:85) containing 0.3‰ formic acid . The methods showed linearity at the range of 0.5–100 µg/mL for each oxiracetam enantiomer. A comprehensive validation process was carried out, covering aspects including linearity, selectivity, carryover, accuracy, precision, interferences, matrix effect, recovery, dilution integrity and stability in matrix and solution. The validated methods were successfully applied to quantifying R-Oxiracetam and S-Oxiracetam in human plasma, urine, and feces of 12 healthy subjects treated with either a single dose of 2 g S-Oxiracetam injection or 4 g Oxiracetam injection in a phase-I clinical trial . There was no significant difference for plasma pharmacokinetic parameters of S-Oxiracetam between the two regimens ( P＞0.05 ). The S-Oxiracetam and Oxiracetam were primarily eliminated through urine in their original form, with cumulative excretion rates of 92.16% and 85.92%, respectively, within 24 h after administration. Enantiomers interconversion was not observed in the plasma, urine, or feces. The results of this study suggest that replacing 4 g Oxiracetam injection with 2 g S-Oxiracetam injection could offer clinical benefits by lowering the dosage and mitigating potential risks, based on the pharmacokinetic characteristics.
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2021
·Vol. 35
·期 7
·e5093
·
IF 1.902
Wei Wu,Rui Cheng,Zhenzhou Jiang,Luyong Zhang,Xin Huang
A rapid and specific UPLC–MS/MS method with a total run time of 3.5 min was developed for the determination of pravastatin, fexofenadine, rosuvastatin, and methotrexate in rat primary hepatocytes. After protein precipitation with 70% acetonitrile (containing 30% H 2 O), these four analytes were separated under gradient conditions with a mobile phase consisting of 0.03% acetic acid (v/v) and methanol at a flow rate of 0.50 mL/min. The linearity, recovery, matrix effect, accuracy, precision, and stability of the method were well validated. We evaluated drug–drug interactions based on these four compounds in freshly suspended hepatocytes. The hepatic uptake of pravastatin, fexofenadine, rosuvastatin, and methotrexate at 4°C was significantly lower than that at 37°C, and the hepatocytes were saturable with increased substrate concentration and culture time, suggesting that the rat primary hepatocyte model was successfully established. Triptolide showed a significant inhibitory effect on the hepatic uptake of these four compounds. In conclusion, this method was successfully employed for the quantification of pravastatin, fexofenadine, rosuvastatin, and methotrexate and was used to verify the rat primary hepatocyte model for Oatp1, Oatp2, Oatp4, and Oat2 transporter studies. Then, we applied this model to explore the effect of triptolide on these four transporters.
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MICROCHIMICA ACTA
·
2017
·Vol. 184
·期 8
·2981-2990
·
IF 4.58
Wang Ting,Liu Siyu,Gao Guihua,Zhao Pan,Lu Nan,Lun Xiaowen,Hou Xiaohong
The authors describe a method for magnetic solid phase extraction (MSPE) combined with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for the quantitation of eight non-steroidal anti-inflammatory drugs (NSAIDs) in wastewater and environmental water samples. Specifically, the NSAIDs were directly extracted by using a magnetic nanocomposite of type Fe 3 O 4 /MIL-101(Cr) (Matérial Institute Lavoisier, MIL) from 50 mL water samples without any further cleanup. The effects of the amount of adsorbent, pH value, salt concentration, ultrasonic extraction time, desorption solvent nature and volume and desorption time were investigated. Under the optimal conditions, UPLC-MS/MS based detection resulted in the following figures of merit: (a) Linear calibration plots that typically extend from 0.1 (0.2, 0.05, 0.02) to 50 μg·L −1 , depending on the compound; (b) detection limits between 3 to 60 ng·L −1 ; and (c), recoveries varying from 81.2% to 116.8% with relative standard deviations between 0.4% and 10.8%. The adsorption of NSAIDs on Fe 3 O 4 /MIL-101(Cr) was characterized by adsorption isotherms, kinetics and thermodynamics studies and provides a deeper insight into the adsorption mechanism. Compared to other method for pretreatment and preconcentration of NSAIDs, the new method is more rapid, sensitive, accurate and eco-friendly. The method was successfully applied to the determination of the NSAID residues in a variety of real environmental and wastewater samples.
Schematic of a method for determination of non-steroidal anti-inflammatory drugs (NSAIDs) in environmental water by magnetic solid phase extraction based on Fe 3 O 4 /MIL-101(Cr) combined with UPLC-MS/MS. The adsorption mechanism of NSAIDs on Fe 3 O 4 /MIL-101(Cr) was studied.
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MICROCHEMICAL JOURNAL
·
2024
·
IF 4.9
Weihang Lu,Tao Chen,Cheng Shen,Denglang Zou,Juyuan Luo,Shuo Wang,Zhibo Song,Jing Jia,Yulin Li
In the present study, an efficient strategy has been established for rapid screening of potential α-glucosidase inhibitors from the waste leaves of Rheum tanguticum by activity-oriented extraction and enrichment optimization, UPLC-QTOF-MS/MS, molecular docking, and in vitro validation. With α-glucosidase inhibitory activity as the evaluation index, the extraction process was optimized by response surface methodology and the enrichment process by macroporous resins was optimized by adsorption and desorption experiments. The active flavonoids yield was 8.85 mg/g under the optimized extraction conditions. After AB-8 macroporous resins enrichment, the active flavonoids purity increased from 2.89 % to 47.6 %, a 17-fold increase, while the IC 50 of α-glucosidase reduced from 13.97 mg/mL to 412 μg/mL, a 33.9-fold reduction. Thirty-six flavonoids in the active flavonoids fraction were identified by UPLC-QTOF-MS/MS. Molecular docking screening, in vitro activity assay and multispectral approaches verification confirmed the potential of six flavonoids as novel α-glucosidase inhibitors.
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TALANTA
·
2025
·
IF 6.1
Xian Li,Xinxin Wen,Zewei Luo,Xuejun Wang,Yilin Zhang,Jing Wei,Yonghui Tian,Rui Ling,Yixiang Duan
Breast cancer (BC) is the primary cause of cancer-related deaths in women. Currently, the discovery of biomarkers primarily relies on single platform, which might overlook other potential biomarkers and lead to inaccurate diagnoses. This study aims to: (1) expand the detection range of biomarkers through multiple analytical techniques, thereby improving the accuracy of BC diagnosis, and (2) analyze the metabolic pathways of the biomarkers to explore the metabolic mechanisms underlying BC. Urine samples from BC patients and healthy controls were analyzed using two techniques: Ultra-high performance liquid chromatography combined with Quadrupole-Exactive-Orbitrap mass spectrometry (UPLC-Q-Exactive Orbitrap-MS), and headspace solid-phase microextraction combined with gas chromatography-high resolution mass spectrometry (HS-SPME/GC-HRMS). Data from each platform was analyzed independently using both univariate and multivariate statistical approaches to identify candidate biomarkers. Subsequently, a mid-level data fusion approach was applied to integrate the candidate biomarkers identified by each platform. The fused data were used to construct orthogonal partial least squares discriminant analysis (OPLS-DA) models and random forest (RF) models, which were then compared against models based on individual platform. The fused RF and OPLS-DA models demonstrated enhanced diagnostic accuracy compared to the individual model. Integrating GC-HRMS and UPLC-Q-Exactive Orbitrap-MS achieved the best performance, with an AUC value of 0.967, sensitivity of 86.37 %, and specificity of 89.19 %. Metabolic pathway analysis revealed that 10 metabolic pathways exert an impact on BC. Four pathways—pyruvate metabolism, sulfur metabolism, taurine and hypotaurine metabolism, and tyrosine metabolism—were found to be associated with BC in both metabolomics and volatolomics studies, indicating that these pathways play pivotal roles in BC. This study confirmed the potential of merging multi-platforms to enhance the accuracy of BC diagnosis, offering new avenues for understanding the metabolic mechanisms of BC.
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高影响因子
DALTON TRANSACTIONS
·
2023
·Vol. 52
·期 36
·12763-12778
·
IF 4
Qi Wen,Di Li,Chunyan Gao,Yuhang Xue,Lei Wu,Fang Song,Jun Zhou
In this paper, ultra-thin nanofiber PDI was obtained by self-assembly dispersion of commercial PDINH. A novel Co/Ni-MOF-74@PDI Z-scheme heterojunction photocatalyst material was constructed by a simple solvothermal method. XRD, SEM, TEM, FT-IR and other characterization techniques proved the successful preparation of the Co/Ni-MOF-74@PDI Z-scheme heterojunction photocatalyst material. By degrading chlortetracycline hydrochloride, it was found that the photocatalytic activity of Co/Ni-MOF-74@PDI was much higher than that of pure Co/Ni-MOF-74 and PDI. Subsequently, Co/Ni-MOF-74@PDI was used to activate H2O2 to further improve the degradation efficiency of chlortetracycline hydrochloride. It was found that the photocatalytic performance was greatly improved after the addition of 19.6 mM H2O2 to the system, and the degradation rate of chlortetracycline hydrochloride was 87% within 90 min. The electron transfer pathway and H2O2 activation mechanism of the Co/Ni-MOF-74@PDI composite photocatalyst were proved by free radical quenching experiments, electron paramagnetic resonance analysis and X-ray electron spectroscopy. Finally, the easy exfoliation point and degradation pathway of chlortetracycline hydrochloride were studied using density functional theory, UPLC-MS and toxicity evaluation software. It was found that the main active substances were h+, ˙O2, 1O2 and ˙OH, and the toxicity of chlortetracycline hydrochloride and its intermediates was evaluated.
研究领域:
材料科学
·
环境科学
·
光化学
·
催化
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RSC Advances
·
2018
·Vol. 8
·期 16
·8586-8595
·
IF 2.936
Wenwen Zhao,Zongyang Liu,Weiwei Guo,Kui Luo,Jie Yang,Wei Gao,Xia Wu,Xiaoqing Chen
Ilexhainanoside D (IhD) and Ilexsaponin A1 (IsA) are a pair of oleanene- and ursane-type triterpenoid saponins, which are also the main bioactive pharmaceutical ingredients of Ilex hainanensis Merr. with great potential to treat non-alcoholic fatty liver disease (NAFLD). The pharmacokinetics of four representative triterpenoids in mice were investigated in this study, which were IhD, IsA and their major metabolites 3β, 19α-dihydroxyolean-12-ene-24, 28-dioic acid (ID) and Ilexgenin A (IA). A sensitive and accurate UPLC-MS/MS method was developed and validated for the simultaneous quantitative determination of IhD, IsA, ID and IA in control and NAFLD mice plasma after oral administration of the total saponins of I. hainanensis (the contents of IhD and IsA were 41.6% and 54.4%, respectively). The results revealed that the pharmacokinetic behaviors could be changed in NAFLD mice compared with control mice. The area under the plasma drug concentration–time curve and maximum plasma concentrations of IhD and IsA were greatly decreased in the NAFLD mice. However, the main residence time of ID and IA were greatly increased in the NAFLD mice. The results revealed that this method could be used to analyze two pairs of triterpenoid isomers in biological samples.
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高影响因子
FOOD RESEARCH INTERNATIONAL
·
2020
·
IF 4.972
An Peng,Lianzhu Lin,Mouming Zhao
This study aimed at obtaining precise quality control standards to efficiently screen Chrysanthemum morifolium Ramat. ‘ Boju ’ with strong xanthine oxidase (XO) inhibitory activity for developing C. morifolium ‘ Boju ’ extract based-hypouricemic functional food. The results indicated significant differences in volatile and phenolic profiles and XO inhibitory (XOI) activities of 31 batches of C. morifolium ‘ Boju ’ collected in herb/tea market. The minority of C. morifolium ‘ Boju ’ having abundant characteristic monoterpenoids and flavonoid aglycones showed strong XOI activities, while the majority of C. morifolium ‘ Boju ’ possessing few corresponding monoterpenoids and flavonoid aglycones exhibited moderate XOI activities. Seven XOI activity-directly related phenolics and ten XOI activity-indirectly related volatiles were identified by UPLC-ESI-QTOF/MS-based and HS-SPME-GC/MS-based spectrum-effect relationships, respectively. Three flavonoids (luteolin, apigenin and acacetin) identified as key XO inhibitors and four monoterpenoids (filifolone, α-terpineol, thymol and piperitenone) closely related to key XO inhibitors were screened for XOI activity-oriented quality control of C. morifolium ‘ Boju ’.
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