ANALYTICA CHIMICA ACTA
·
2024
·
IF 5.7
Caiming Tang,Yizhe Zhu,Ruifen Zheng,Ling Liu,Yan-Hong Zeng,Xiao-Jun Luo,Bi-Xian Mai
Background N,N′-disubstituted p -phenylenediamine-quinones (PPDQs) are oxidization derivatives of p -phenylenediamines (PPDs) and have raised extensive concerns recently, due to their toxicities and prevalence in the environment, particularly in water environment. PPDQs are derived from tire rubbers, in which other PPD oxidization products besides reported PPDQs may also exist, e.g., unknown PPDQs and PPD-phenols (PPDPs). Results This study implemented nontarget analysis and profiling for PPDQ/Ps in aged tire rubbers using liquid chromatography-high-resolution mass spectrometry and a species-specific algorithm. The algorithm took into account the ionization behaviors of PPDQ/Ps in both positive and negative electrospray ionization, and their specific carbon isotopologue distributions. A total of 47 formulas of PPDQ/Ps were found and elucidated with tentative or accurate structures, including 25 PPDQs, 18 PPDPs and 4 PPD-hydroxy-quinones (PPDHQs). The semiquantified total concentrations of PPDQ/Ps were 14.08–30.62 μg/g, and the concentrations followed the order as: PPDPs (6.48–17.39) > PPDQs (5.86–12.14) > PPDHQs (0.16–1.35 μg/g). Significance The high concentrations and potential toxicities indicate that these PPDQ/Ps could seriously threaten the eco-environment, as they may finally enter the environment, accordingly requiring further investigation. The analysis strategy and data-processing algorithm can be extended to nontarget analysis for other zwitterionic pollutants, and the analysis results provide new understandings on the environmental occurrence of PPDQ/Ps from source and overall perspectives.
研究领域:
环境科学
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分析化学
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产品关联
DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2018
·Vol. 33
·期 2
·e4400
·
IF 1.688
Lihua Zuo,Zhi Sun,Zhenhui Wang,Daling Ding,Tanye Xu,Liwei Liu,Li Gao,Shuzhang Du,Jian Kang,Xiaojian Zhang
Xuebijing injection (XBJI) is a traditional Chinese medicine prescription extracted from five Chinese herbs. Hydroxysafflor yellow A, oxypaeoniflorin, ferulic acid and benzoylpaeoniflorin are the main bioactive ingredients of XBJI. This paper presents an application of ultra-high-performance liquid chromatography–Q–exactive hybrid quadrupole–Orbitrap high-resolution mass spectrometry (UHPLC–Q–Orbitrap HRMS) to quantify four compounds of XBJI in rats various tissues for tissue distribution studies. The analytes were separated on a Waters Acquity UHPLC ® BEH C 18 column with a gradient mobile phase consisting of acetonitrile–water (containing 0.1% formic acid) at a flow rate of 0.2 mL/min. Mass spectrometric detection was performed by parallel reaction monitoring via a heated electrospray ionization source under the negative ionization mode. The method was validated in various tissue samples, and has demonstrated great performance for rapidity, accuracy, high sensitivity and selectivity. It was successfully applied to the tissue distribution studies of XBJI after intravenous administration to rats. It was also the first study to investigate the tissue distribution of XBJI in rats and we found that the concentrations of four compounds were high in kidney, liver, stomach and intestine. The clinical use of XBJI should focus on its pharmacodynamics and safety studies in these tissues.
研究领域:
药理学
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分析化学
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中药学
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产品关联
DOI
PubMed
高影响因子
Frontiers in Pharmacology
·
2021
·
IF 5.811
Yang Wenning,Jiang Xiaoquan,Liu Jingtong,Qi Dongying,Luo Zhiqiang,Yu Guohua,Li Xueyan,Sen Muli,Chen Hongjiao,Liu Wei,Liu Yang,Wang Guopeng
The study of screening active constituents from traditional Chinese medicine (TCM) is important for explicating the mechanism of action of TCM and further evaluating the safety and efficacy effectively. However, detecting and identifying the active constituents from complicated biological samples still remain a challenge. Here, a practical, quick, and novel integrated strategy from in vitro, in situ, in vivo to in silico for rapidly screening the active constituents was developed. Firstly, the chemical profile of TCM in vitro was identified using UPLC-Q Exactive-Orbitrap HRMS. Secondly, the in situ intestinal perfusion with venous sampling (IPVS) method was used to investigate the intestinal absorption components. Thirdly, after intragastric administration of the TCM extract, the in vivo absorbed prototype components were detected and identified. Finally, the target network pharmacology approach was applied to explore the potential targets and possible mechanisms of the absorbed components from TCM. The reliability and availability of this approach was demonstrated using Tongfengding capsule (TFDC) as an example of herbal medicine. A total of 141 compounds were detected and identified in TFDC, and among them, 64 components were absorbed into the plasma. Then, a total of 35 absorbed bioactive components and 50 related targets shared commonly by compounds and gout were integrated via target network pharmacology analysis. Ultimately, the effects of the absorbed components on metabolism pathways were verified by experiments. These results demonstrated that this original method may provide a practical tool for screening bioactive compounds from TCM treating particular diseases. Furthermore, it also can clarify the potential mechanism of action of TCM and rationalize the application of TFDC as an effective herbal therapy for gout.
研究领域:
中药学
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药理学
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生物信息学
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药学
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产品关联
DOI
PubMed
高影响因子
PLoS One
·
2024
·Vol. 19
·期 6
·e0304852
·
IF 2.9
Jianting Ouyang,Danyao Lin,Xuesheng Chen,Yimeng Li,Qin Liu,Delun Li,Haohao Quan,Xinwen Fu,Qiaoru Wu,Xiaowan Wang,Shouhai Wu,Chuang Li,Yi Feng,Wei Mao
Background
Known for its strong diuretic properties, the perennial herbaceous plant Orthosiphon stamineus Benth. is believed to preserve the kidney disease. This study compared the boiling water extract with powdered Orthosiphon stamineus Benth. and used a highly sensitive and high resolution UHPLC-Q-Exactive-Orbitrap-HRMS technology to evaluate its chemical composition.
Results
Furthermore, by monitoring the absorption of prototype components in rat plasma following oral treatment, the beneficial ingredients of the Orthosiphon stamineus Benth. decoction was discovered. Approximately 92 substances underwent a preliminary identification utilizing relevant databases, relevant literature, and reference standards. As the compound differences between the powdered Orthosiphon stamineus Benth. and its water decoction were analyzed, it was found that boiling produced additional compounds, 48 of which were new. 45 blood absorption prototype components and 49 OS metabolites were discovered from rat serum, and a kidney tissue homogenate revealed an additional 28 prototype components. Early differences in the distribution of ferulic acid, cis 4 coumaric acid, and rosmarinic acid were shown using spatial metabolomics. It was elucidated that the renal cortex region is where rosmarinic acid largely acts, offering a theoretical foundation for further studies on the application of OS in the prevention and treatment of illness as well as the preservation of kidney function.
Significance
In this study, UHPLC–Q Exactive Orbitrap–HRMS was employed to discern OS’s chemical composition, and a rapid, sensitive, and broad-coverage AFADESI-MSI method was developed to visualize the spatial distribution of compounds in tissues.
研究领域:
植物化学
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药理学
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分析化学
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产品关联
DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2026
·
IF 5.2
Ying-Fang Jian,Mei Li,Hai-Sha Liu,Jin-Kuang Jiang,Dong-Mei Chen,Xiu-Fang Yan,Chao Kang,Ya-Juan Liu
Apple branch canker, caused by Botryosphaeria dothidea , poses a serious threat to apple production worldwide. Despite its economic importance, current understanding and analysis techniques of the infection dynamics and host defense responses remains limited. Here, an in situ , label-free, high-throughput, and precise imaging method based on confocal Raman microspectroscopic imaging coupled with chemometrics was developed to characterize key defensive constituents, including lipids, lignin, phenols, cellulose, hemicellulose, and pectin, within the cuticle and cell wall, and to monitor their spatiotemporal dynamics across the epidermis and cortex. During infection, lignin of the cuticle in epidermis initially decreased while lipids and phenols increased; Defensive components of cell wall in the cortex decreased and then increased by 3 days; All these constituents decreased by 5 days, leading to disease symptoms. Furthermore, to gain a systems-level understanding, untargeted metabolomics using UPLC–Q–Orbitrap–MS and machine learning screened 2090 differential metabolites (including phenylpropanoids and polyketides, organic heterocyclic compounds, lipids, and lipid-like molecules), and revealed significantly enriched metabolic pathways associated with defense activation ( e.g. , isoquinoline alkaloid biosynthesis, flavonoid biosynthesis). Additionally, a rapid, non-destructive diagnostic platform integrating Raman spectroscopy with machine learning achieved early detection of apple branch canker with an overall accuracy of 97.2%. Collectively, this integrated multi-technology strategy provides new insights into the pathogenicity and defense responses of fruit trees and establishes a non-destructive tool for early disease diagnosis.
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产品关联
DOI
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2026
·
IF 3.4
Lin Chen,Han Huang,Zhonge Li
Four biomarkers were identified by UPLC-Q/Orbitrap HRMS and PLS-DA analysis. • Classification models were built with machine learning and four biomarkers. • The optimal decision tree model can effectively identify adulterated moxa floss. Detecting adulteration in closely related herbal medicines is a challenge for quality control and market standardization. This study aimed to identify whether Artemisia mongolica floss was adulterated into moxa floss. First, ultra-performance liquid chromatography coupled with quadrupole Orbitrap high-resolution mass spectrometry was employed to analyze the chemical compositions of moxa floss and Artemisia mongolica floss. Combined with partial least squares discriminant analysis, four key differential biomarkers were identified. Subsequently, high-performance liquid chromatography (HPLC) methods were established for these biomarkers, providing the data foundation for subsequent adulteration discrimination model development. Moreover, four machine learning classification models were constructed: logistic regression, decision tree, random forest, and extreme gradient boosting to compare their ability to identify adulterated samples. The results indicated that the decision tree model exhibited strong generalization capability and stability. Based on the established HPLC method and decision tree model, the ratio range of peak areas of the biomarker 5-hydroxy-3′,4′,6,7-tetramethoxyflavone to eupatilin or jaceosidin can be used as an indicator to effectively identify adulterated samples. In summary, the study established an analytical strategy for identifying specific markers, thereby facilitating practical discrimination in cases of moxa floss adulteration.
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DOI
PubMed
高影响因子
ANALYTICAL CHEMISTRY
·
2025
·
IF 6.7
Tian Tian,Xi Chen,Li Liu,Xueqi Liang,Xiaojun Deng
The current limited understanding of small bioactive peptide metabolism hinders effective doping control. A primary challenge lies in distinguishing suspicious features from extensive mass spectral datasets contaminated by biological matrix interference and background noise. In this study, we introduce a strategy integrating in silico prediction and nontargeted data mining to achieve more comprehensive metabolic profiling through ultrahigh-performance liquid chromatography–high-resolution mass spectrometry (UHPLC-HRMS). The strategy operates by identifying and applying chemical similarity (CSIM) rules of peptides (such as LC/MS behaviors and specific biotransformation) to mine unknown metabolites. With this strategy, a semiautomated workflow utilizing computational software and custom script was constructed and applied to the human liver microsomal metabolism of two significant kisspeptin analogues with doping potential (TAK-448 and TAK-683). The characteristic behaviors induced by CSIM enabled effectively in-depth data mining from redundant background signals, leading to the identification of 13 metabolites (three were validated via synthetic standards) and two uncommon biotransformation pathways (N-terminal vinylation and N-terminal carboxylation) for both investigated compounds. Notably, the two biotransformation pathways offered an innovative perspective on small peptide metabolism, which was further confirmed in rats, and produced two promising long-term metabolites for monitoring doping abuse. Further drug activity evaluation indicated higher or retained performance-enhancing effects of these metabolites, alerting doping control subjects to pay attention to more information. The study provided the first comprehensive characterization of the metabolic profiles of TAK-448 and TAK-683, while also offering an effective tool for metabolism research on small peptide doping agents.
研究领域:
分析化学
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药学
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代谢组学
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兴奋剂检测
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生物信息学
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DOI
PubMed
高影响因子
INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES
·
2023
·
IF 8.2
Qianqian Feng,Wei Yang,Zhiyun Peng,Guangcheng Wang
Oxalis corniculate L. ( O. corniculate ) was used to treat diabetes in Chinese folk as a popular tea drink. In this work, 31 compounds from O. corniculate were screened and identified as potential α-Glucosidase inhibitors (α-GIs). Among them, 6 compounds displayed stronger inhibitory activity than acarbose (IC 50 = 212.9 ± 5.98 μg/mL). Especially, the most effective compounds quercetin (Qu, IC 50 = 4.70 ± 0.40 μg/mL) and luteolin (Lu, IC 50 = 15.72 ± 0.75 μg/mL) inhibited α-Glu in competitive and mixed manners, respectively. Moreover, fluorescence quenching , circular dichroism (CD), and molecular docking study revealed that they can arouse the changes in the secondary structure and hydrophobic micro-environment of the enzyme mainly through a hydrophobic binding. Furthermore, it was observed that oral administration of Qu (20 mg/kg) can significantly reduce postprandial blood glucose (PBG) levels in mice vs. the control group. To sum up, the above research confirmed that O. corniculate could prevent and treat postprandial hyperglycemia as a good tea drink, and the plant was an excellent source to obtain natural α-GIs.
研究领域:
药理学
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生物化学
·
分析化学
·
药物化学
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产品关联
DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2026
·
IF 5.2
Yue Sun,Juntao Wang,Shiqiong Chen,Qin Yang,Sixin Liu,Congfa Li
This study presents a comprehensive characterization and comparison of polyphenols in Alpiniae oxyphyllae fructus extracted using ultrasound-assisted deep eutectic solvents (DESs) versus traditional solvents. The contents of total polyphenols in Choline chloride -malic acid (ChCl-MA) (1:1) , ChCl-MA (1:2) , L-proline-Lactic acid (Pro-LA) (1:1) , Pro-LA (1:3) , and L-proline-citric acid (Pro-CA) (1:3) extracts were the highest, ranging from 17.67 to 19.37 mg/g, and were significantly higher than those in water extract (10.35 mg/g) and ethanol extract (14.78 mg/g) ( p < 0.05). Pro-LA extract exhibited high levels of 3,4-dihydroxybenzoic acid and protocatechualdehyde, and possessed strong antioxidant activity. Density functional theory (DFT) calculations indicated that the mechanism of DESs' efficient extraction of polyphenols was mainly reflected in the unique structural configuration of Pro-LA, which facilitated the formation of strong hydrogen bonds with the hydroxyl functional groups of polyphenols, enhancing the intermolecular interaction, and thus improving the extraction efficiency. Our study provided a novel approach for the efficient extraction of plant polyphenols.
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DOI
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2017
·
IF 3.255
Lihua Zuo,Qiuyue Zhong,Zhenhui Wang,Zhi Sun,Lin Zhou,Zhuolun Li,Tanye Xu,Yingying Shi,Jinfa Tang,Shuzhang Du,Xiaojian Zhang
Xuebijing injection (XBJ) is a traditional Chinese herbal prescription widely used in the treatment of sepsis. Extensive studies revealed that the major bioactive constituents of XBJ injection, including phenolic acids, flavonoids, monoterpene glycosides, lactones and organic acids, play an important role in the treatment. In this study, a rapid, sensitive and accurate ultra high performance liquid chromatography – Q Exactive hybrid quadrupole – orbitrap high-resolution accurate mass spectrometry (UHPLC-Q-Orbitrap HRMS) method was developed for simultaneous determination of twelve bioactive compounds in rat plasma after intravenous administration of XBJ injection. A gradient elution for separation was achieved on a waters ACQUITY UHPLC ® BEH C 18 column (2.1 mm × 50 mm, 1.7 μm) column with acetonitrile-water (containing 0.1% formic acid) as mobile phase at a flow rate of 0.2 mL/min. All compounds and IS were monitored by parallel reaction monitoring assay both in positive and negative ion mode. The developed method was validated for intra-day and inter-day accuracy and precision whose values fell in the acceptable limits. Extraction recoveries at three levels of QC concentrations were all more than 80% for all compounds and IS, and matrix effects were found in the range of 80.0–120.0%. Stability results showed that all analytes were stable at the investigated conditions. The validated method was successfully applied to a pharmacokinetic study of Xuebijing injection following intravenous administration of 2.5, 5.0, 10.0 mL/kg to rats respectively. And the result indicated that the pharmacokinetic behavior of XBJ injection is positively related to dosage at the range of 2.5–10 mg/kg. This study will provide a meaningful basis for evaluating the rationality of XBJ injection for clinical application.
研究领域:
中药学
·
分析化学
·
药理学
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产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2023
·
IF 8.8
Tongtong Jia,Shaolun Ouyang,Wenrui Chen,Ting Zhang,Mengqi Lu,Xiuying Zhou,Hongtao Lei,Xiaoqun Wei
To get rid of the singularity of the detection of veterinary drug residues in liquid milk, a high-throughput determination was developed for 126 VDRs in 17 categories in liquid milk based on the one-step extraction coupled with LC-HRMS (UPLC-Q-Exactive-Orbitrap-MS). The results showed that adding 2.5 mL of 0.1 mol/L Na2EDTA-McIlvaine in acetonitrile-methanol extractant (50:50, V/V) could effectively improve the response intensity of veterinary drug residues in liquid milk, reduce the matrix effect and eliminate the need for expensive SPE purification. The established external standard quantitative method has a LOD of 0.01–0.30 μg/L for all categories of veterinary drug residues, good linearity in the concentration range of LOQ of 0.03–1.00 μg/L, and correlation coefficients (r 2 ) were all greater than 0.995. The spike recoveries at all three levels were between 80.30% and 119.95%. The positive detection rate of this method in 128 actual samples was 8.59%.
研究领域:
分析化学
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食品科学
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兽医学
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产品关联
DOI
PubMed
高影响因子
Analytical Methods
·
2022
·Vol. 14
·期 47
·4990-5000
·
IF 3.532
Xiangyu Zhang,Yaojuan Chu,Mengli Wang,Yingying Shi,Lihua Zuo,Zhuolun Li,Jiyun Liu,Jian Kang,Shuzhang Du,Bing Li,Zhi Sun,Xiaojian Zhang
Mai-Luo-Shu-Tong pill is an effective traditional Chinese medicine formula for the treatment of superficial thrombophlebitis, but it was insufficiently chemically scrutinized. In this study, the mass spectral data of Mai-Luo-Shu-Tong pill were acquired by ultra-high performance liquid chromatography coupled with Q Exactive hybrid Quadrupole-Orbitrap high resolution mass spectrometry. Then, a data mining strategy combining multiple data processing methods was used to identify chemical constituents in Mai-Luo-Shu-Tong pill by constructing a database of precursor ions and summarizing the mass spectral fragmentation behaviors. As a result, a total of 211 compounds including 70 flavonoids, 56 terpenoids, 37 phenolic acids and 48 others were identified in positive and negative ion modes. Among them, 66 compounds have passed comparison verification with reference standards, 145 compounds were identified based on the data mining strategy combining the characteristic cleavage behaviour of homologous compounds and fragment ions and 4 compounds were potentially new compounds. This study provides a database for quality evaluation and further study of Mai-Luo-Shu-Tong pill in vivo. Moreover, it provides a reference for the characterization of the chemical constituents of other traditional Chinese medicine formulae.
研究领域:
中药化学
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分析化学
·
药学
✓ 已验证
DOI
高影响因子
危险品化学品经营许可证（带存储）