Chemosensors
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2023
·Vol. 11
·期 3
·165
·
IF 4.2
Yi Lv,Feng-Lian Ma,Jia-Nan Wang,Yao Zhang,Yuan Jiang,Qian Ge,Yong-Jie Yu
The time involved and the high economic cost of using oak barrels to age wines have led to a significant price difference compared to non-oak barrel aged wines and may lead to some fraudulent sales in the market. In this study, an untargeted metabolomic strategy was developed to detect the metabolite composition of oak barrel aged and non-oak barrel aged wines in both positive and negative ion modes by using UHPLC–HRMS combined with the recently developed chemometric method AntDAS. The results of partial least squares discrimination analysis (PLS-DA) showed that the samples were characterized into two categories. Finally, 51 compounds were identified in positive ion mode, while 26 compounds were identified in negative ion mode. The results indicate that combining UHPLC–HRMS with AntDAS can reveal the material basis of wines and has excellent potential to differentiate between oak barrel aged and non-oak barrel aged wines.Keywords:oak barrel aged wines;UHPLC-HRMS;AntDAS;chemometrics
研究领域:
食品科学
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分析化学
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化学计量学
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DOI
高影响因子
JOURNAL OF HAZARDOUS MATERIALS
·
2022
·
IF 14.224
Xiao Wang,Ya Zhao,Xin Qi,Tiantian Zhao,Xiupin Wang,Fei Ma,Liangxiao Zhang,Qi Zhang,Peiwu Li
Aflatoxins seriously threaten human health and food safety, and early warning benefits the reasonable use of control measures to reduce aflatoxin contamination. In this study, a novel method for quantifying aflatoxins and their precursors in the aflatoxin biosynthesis pathway was developed by combining ultra-high performance liquid chromatography high-resolution mass spectrometry (UHPLC-HRMS) with quantitative analysis of multi-components by a single marker (QAMS). The stability of the relative correction factor (RCF) of QAMS was then systematically evaluated. The validation results showed that the relative deviation (RD) between QAMS and the external standard method (ESM) was less than 11.7%, indicating that the established QAMS method could replace ESM without the use of reference standards. This method was successfully employed to compare the time-course changes of metabolites in the aflatoxin biosynthesis pathway of Aspergillus flavus and Aspergillus parasitica. As a result, the precursors of (1'S,5′R)−5′-Hydroxyaverantin (HAVN) and Versicolorin B (VerB) could be used as potential markers for the early warning of aflatoxin contamination. This study provided a quantitative method of aflatoxins and their precursors in the biosynthesis pathway, and may serve as a reference for the extension of quantitative studies on other metabolic pathways.
研究领域:
食品安全
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分子生物学
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DOI
PubMed
高影响因子
Foods
·
2021
·Vol. 11
·期 1
·93
·
IF 4.35
Chenling Qu,Zhuozhen Li,Xiupin Wang
Aspergillus flavusis a common contaminant in grain, oil and their products. Its metabolite aflatoxin B1(AFB1) has been proved to be highly carcinogenic. Therefore, it is of great importance to find possible antifungal substances to inhibit the growth and toxin production ofAspergillus flavus. Carvacrol (CV) was reported as a potent antifungal monoterpene derived from plants. In this paper, the antifungal effects and mechanism of CV onAspergillus flavuswere investigated. CV was shown good inhibition on the growth ofAspergillus flavusand the production of AFB1. CV used in concentrations ranging from 0, 50, 100 and 200 μg/mL inhibited the germination of spores, mycelia growth and AFB1production dose-dependently. To explore the antifungal mechanism of CV onAspergillus flavus, we also detected the ergosterol content ofAspergillus flavusmycelia, employed Scanning Electron Microscopy (SEM) to observe mycelia morphology and utilized Ultra-High-Performance Liquid Chromatography-High-Resolution Mass Spectrometry (UHPLC-HRMS) to explore the lipidome profiles ofAspergillus flavus. The results showed that the production of ergosterol of mycelia was reduced as the CV treatment concentration increased. SEM photographs demonstrated a rough surface and a reduction in the thickness of hyphae inAspergillus flavustreated with CV (200 µg/mL). In positive ion mode, 21 lipids ofAspergillus flavusmycelium were downregulated, and 11 lipids were upregulated after treatment with 200-µg/mL CV. In negative ion mode, nine lipids ofAspergillus flavusmycelium were downregulated, and seven lipids upregulated after treatment with 200-µg/mL CV. In addition, the analysis of different lipid metabolic pathways between the control and 200-µg/mL CV-treated groups demonstrated that glycerophospholipid metabolism was the most enriched pathway related to CV treatment.Keywords:Aspergillus flavus;carvacrol;untargeted lipidomics;ultra-high-performance liquid chromatography-high-resolution mass spectrometry (UHPLC-HRMS);antifungal activity
研究领域:
微生物学
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药理学
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分析化学
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DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2024
·
IF 3.1
Songze Wang,Xin Zhou,Xin Wang,Shengyu Cheng,Xi-Ling Li,Jun Nan,Jun Zhe Min
Human hair is a non-invasive biological sample that is easy to collect and store and can reflect long-term body health. However, the correlation between DL-amino acids and metabolic diseases in hair samples has not been studied. Therefore, we propose a novel UHPLC-HRMS method for analyzing seven free chiral amino acids (DL-Thr, DL-Glu, DL-Ala, DL-Val, DL-Pro, DL-Leu, and DL-Phe) simultaneously in hair samples by derivatization of chiral probe 4-(N,N-dmethylaminosulfonyl)-2,1,3-benzoxadiazole-trans-2-methyl-L-proline (DBD-M-Pro) labeled with targeted amino functional groups. Gradient elution was carried out using an ACQUITYTM BEH C18 (100×2.1 mm,1.7 μm) column with a mobile phase of 0.15 % formic acid (FA) in 10 mM ammonium acetate (CH 3 -COONH 4 ) and 0.2 % FA in acetonitrile. The labelled DL-amino acid diastereoisomers could be completely separated, with a resolution (Rs) of 1.59–11.44. These amino acids show a strong linear correlation within the range of 3.1–99.2 pmol (R 2 ≥ 0.9990). Intraday and interday precision was 1.87 %–14.87 %. The average recovery was 96.12 %–105.33 %. The limit of detection (LOD) ranged from 0.29 to 2.11 pmol. We then employed the method to determine the concentration of free chiral amino acids in hair samples from 30 healthy volunteers (HVs) and 30 diabetes patients (DPs). Male diabetes patients had significantly higher levels of L-Thr, L-Val, L-Leu ( p < 0.05), and D-Ala ( p < 0.01) in their hair samples than male healthy volunteers and female diabetes patients had significantly higher levels of D-Ala ( p < 0.05) in their hair samples than female healthy volunteers. This is the first study to confirm the feasibility of using free DL-amino acids in human hair as potential biomarkers for diabetes.
研究领域:
分析化学
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代谢组学
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临床化学
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产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2024
·
IF 8.5
Huan Liu,Jingyu Li,Yuping Zhang,Lin Li,Hansheng Gong,Lixuan Tan,Peng Gao,Pi Li,Jiangtao Xing,Bin Liang,Jianxun Li
Lipids are key aroma contributors in meat products. However, the role of different lipids in the presence of aroma compounds in roasted pigeons has not been studied. The formation of aroma compounds and lipids during the circulating non-fried roasting of pigeons was investigated. The results presented that 18 aroma compounds, including 5-methy-2,3-diethylpyrazine, were identified as key aroma compounds. A total of 6324 lipids were classed into 47 categories, such as phosphatidylcholine (PC), phosphatidylethanolamine (PE), and triglyceride (TG). Nine lipids, containing PA(P-20:0/22:4(7Z,10Z,13Z,16Z)) and LPC 16:0-SN1, showed promise as potential biomarkers for discriminating differential pigeons using OPLS-DA. PC (13.76%), TG (13.58%), and their products were major lipids, among which TG 16:0 16:0 18:2, LPC 18:2-SN1, and PC 18:1_18:1 played a crucial role in the presence of aroma compounds. Interestingly, the linoleic acid , an important aroma contributor, was predominantly bonded to the sn-2 position of phospholipid and sn-3 position of neutral lipids.
研究领域:
食品科学
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分析化学
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产品关联
DOI
PubMed
高影响因子
ANALYTICAL CHEMISTRY
·
2026
·
IF 7.3
Jun-Yi Zhou,Yan Zhang,Lu-Lu Wen,Yun Du,Wan-Cheng Zheng,Xiao-Xuan Duan,Miao Qu,Hai-Yu Zhao,Jian-Bo Wan
Abstract Regiospecific analysis of monoacylglycerols (MAGs) remains challenging because of their low endogenous abundance, the limited availability of regioisomeric standards, and rapid acyl migration between the sn-1 and sn-2 positions during sample handling. Here, we report an UHPLC–HRMS platform integrating chemical stabilization with retention-time prediction for confident profiling of MAG regioisomers in biological samples. Derivatization with 4-pyridineboronic acid (4-PyBA) selectively forms cyclic boronate esters with the glycerol cis-diol moiety, thereby suppressing acyl migration, enhancing electrospray ionization efficiency, and generating characteristic diagnostic ions. To minimize reliance on authentic standards, a three-dimensional quantitative structure–retention relationship (3D-QSRR) model was developed to predict chromatographic retention across structurally diverse MAGs. In parallel, a homologous series of fatty acid 1,2-pentanediol monoesters was synthesized as retention calibrants to correct retention time (RT) drift and improve method robustness. These components were integrated into a targeted parallel reaction monitoring (PRM) workflow supported by an in-house database of 288 annotated sn-1 and sn-2 MAGs. Application of this strategy to serum, brain, colon, and fecal samples from APP/PS1 mice and to serum samples from individuals with Alzheimer’s disease (AD) enabled the confident annotation of 118 endogenous MAGs, including 68 MAGs not currently catalogued in major public databases. Collectively, this integrated platform improves structural confidence and analytical robustness and establishes a transferable framework for regioisomer-resolved analysis of labile glycerolipids.
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DOI
高影响因子
ANALYTICA CHIMICA ACTA
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2024
·
IF 5.7
Jun-Yi Zhou,Yan-Qing Chen,Guang Hu,Haiyu Zhao,Jian-Bo Wan
Background N-acylethanolamines (NAEs) are a class of naturally occurring bioactive lipids that play crucial roles in various physiological processes, particularly exhibiting neuroprotective and anti-inflammatory properties. However, the comprehensive profiling of endogenous NAEs in complex biological matrices is challenging due to their low abundance, structural similarity and the limited availability of commercial standards. Here, we propose an integrated strategy for comprehensive profiling of NAEs that combines chemical derivatization and a three-dimensional (3D) prediction model based on quantitative structure-retention time relationship (QSRR) using liquid chromatography coupled with high-resolution tandem mass spectrometry (LC-HRMS). Results After acetyl chloride (ACC) derivatization, the detection sensitivity of NAEs was significantly improved. We developed a QSRR prediction model to construct an in-house database for 141 NAEs, encompassing information on RT, MS 1 ( m/z ), and MS/MS spectra. Propargylamine-labeled fatty acids were synthesized as RT calibrants across various analytical conditions to enhance the robustness of the RT prediction model. NAEs in biological samples were then in-depth profiled using parallel reaction monitoring (PRM) acquisition. This integrated strategy identified and annotated a total of 50 NAEs across serum, hippocampus and cortex tissues from a 5xFAD mouse model of Alzheimer's disease (AD). Notably, the levels of polyunsaturated NAEs, particularly NAE 20:5 and NAE 22:6, were significantly decreased in 5xFAD mice compared to WT mice, as confirmed by accurate quantitation using ACC- d 0 / d 3 derivatization. Significance Our integrated strategy exhibits great potential for the in-depth profiling of NAEs in complex biological samples, facilitating the elucidation of NAE functions in diverse physiological and pathological processes.
研究领域:
生物化学
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医学
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分析化学
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DOI
PubMed
高影响因子
Scientific Reports
·
2025
·Vol. 15
·期 1
·1-18
·
IF 3.9
Ma Qingkun,Zhang Mei,Fan Yongshuai,Zhao Han,Wang Kun,Wang Xiaojing,Mu Yanling
Thiol compounds can serve as markers for the antioxidant and prognostic status of lymphoma, playing a crucial role in early tumor diagnosis. However, their high polarity and lack of chromophores pose challenges for multivariate analysis. This study aims to measure thiols associated proteins and develop novel diagnostic models in serum and cerebrospinal fluid from PCNSL to verify potential association and early warning effectiveness. A highly sensitive and selective method was established for simultaneous determination of 7 different thiols and 340 related proteins based on self-developed mass spectrometry probe, Br-OTPP labeled by UHPLC-HRMS. Furthermore, a novel PCNSL monitoring model was developed based on different those combined with machine learning algorithm. Thiols has good linear relationship with correlation coefficients ≥ 0.9995 and suitable precision with inter-day and intra-day coefficients variation was 2.08–5.49% and 1.58–5.53%. Satisfactory accuracy with recoveries between 85.28 and 97.88% was observed. The limit of detection (S/ N = 3) was 0.8-9.0 fmol. Ultimately, this method greatly improves discrimination efficiency of model with accuracy of 98.83%. The proposed method could successfully apply into measurement of thiols associated proteins and development of multi-omics clinical evaluation model for PCNSL patients.
研究领域:
分析化学
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临床医学
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肿瘤学
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生物化学
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蛋白质组学
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医学诊断
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产品关联
DOI
PubMed
高影响因子
Drug Testing and Analysis
·
2026
·
IF 2.6
Tian Tian,Xi Chen,Xiaojun Deng
The gastric-emptying and satiety effects of semaglutide may lead to its misuse by athletes in weight-class sports, especially as the approved oral formulation is more convenient than subcutaneous injections. This study aimed to establish a simple ultrahigh-performance liquid chromatography-high resolution mass spectrometry (UHPLC-HRMS) method for monitoring semaglutide abuse based on urinary metabolites U6 and U7, and elucidate the urinary excretion profile of the oral formulation. Multidimensional optimization determined three key factors for reliable trace detection (recovery > 90%), with enhanced hydrophobic interactions dominating the enrichment process: (i) the adsorbent, (ii) the loading pH, and (iii) the washing solvent. Orbitrap-HRMS operating in dual acquisition modes enabled both specific identification and retrospective analysis. Systematic qualitative and quantitative validation was performed, and a single oral microdose of semaglutide (3 mg) was administered to a healthy volunteer, followed by continuous urine collection for 1 week. The optimized method provided satisfactory sensitivity (limit of detection of 0.03 ng/mL) and quantitative performance (linearity range: 0.1–20 ng/mL, R 2 > 0.995; accuracy > 85%) for both U6 and U7. Excretion profiling of 25 postdose samples showed that U6 and U7 were first detectable at 21 h, peaked at 0.15 and 0.10 ng/mL, respectively, and remained detectable for up to 28 h. Additionally, five abundant metabolites of the absorption enhancer salcaprozate sodium were identified (detection window up to 7 days), serving as sensitive screening indicators for oral semaglutide. These findings demonstrate the effectiveness of the developed method and provide the first perspective on the urinary excretion profile of oral semaglutide.
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DOI
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2025
·Vol. 39
·期 4
·e70038
·
IF 1.7
Mengjiao Li,Fuqiang Liu,Lulu Guo,Wu Fan,Jiazhong Wang,Binbin Lu,Guangfeng Hong,Wenjuan Zhang,Shu Tian,Jian Mao,Jianping Xie
Cordycepin, a natural adenosine derivative, exhibits multiple pharmacological effects on organisms. However, its distribution and metabolic characteristics have not been fully elucidated in vivo. In this study, ultra-high liquid chromatography tandem high-resolution mass spectrometry (UHPLC-HRMS/MS) was used to investigate the pharmacokinetic characteristics and effects of cordycepin on endogenous adenosine and inosine. Microdialysis was used for real-time monitoring of unbound drug in brain and blood, whereas conventional tissue homogenate methods assessed distribution in various tissues. Results showed that the distribution pattern of cordycepin was as follows: kidney > liver > heart > lung > spleen > brain. Cordycepin administration significantly altered the levels of adenosine and inosine in heart and liver. Synchronous microdialysis sampling for the pharmacokinetic profile indicated that cordycepin was rapidly consumed and 3′-deoxyinosine was generated as the main metabolite. The C max values of cordycepin in the rat blood and brain after exposure (10 mg/kg, i.p.) were 7.8 and 5.4 ng/mL, respectively. Mean residence time in blood and brain was 102.2 and 137.0 min, respectively. Inhibition of adenosine deaminase by racemic 9-(2-hydroxy-3-nonyl) adenine hydrochloride (EHNA) enhanced cordycepin levels in the blood. This work provides a solid basis for understanding the metabolism of cordycepin and its pharmacological effects.
研究领域:
药理学
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分析化学
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生物化学
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产品关联
DOI
PubMed
高影响因子
FOOD RESEARCH INTERNATIONAL
·
2024
·
IF 7
Jingyu Li,Yuping Zhang,Renyu Zhang,Rujie Yang,Qianli Ma,Zhongshuai Wang,Pi Li,Jiangtao Xing,Peng Gao,Huan Liu,Hansheng Gong
Lipids are the key matrix for the presence of odorants in meat products. The formation mechanism of odorants of air-fried (AF) pork at 230 °C was elucidated from the perspectives of lipids and heat transfer using physicochemical analyses and multidimensional statistics. Twenty-nine key aroma compounds were identified, with pyrazines predominantly contributing to the roasty aroma of air-fried roasted pork. Untargeted lipidomics revealed 1184 lipids in pork during roasting, with phosphatidylcholine (PC), phosphatidylethanolamine (PE), and triglyceride (TG) being the major lipids accounting for about 60 % of the total lipids. TG with C 18 acyl groups, such as TG 16:1_18:1_18:2 and TG 18:0_18:0_20:3, were particularly significant in forming the aroma of AF pork. The OPLS-DA model identified seven potential biomarkers that differentiate five roasting times, including PC 16:0_18:3 and 2-ethyl-3,5-dimethylpyrazine. Notably, a lower specific heat capacity and water activity accelerated heat transfer, promoting the formation and retention of odorants in AF pork.
研究领域:
食品科学
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分析化学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2024
·
IF 2.8
Tong Zhang,Zhuoqian Guo,Tao Ma,Shanlan Li,Ziqi Dai,Yujin Luo,Feng Gao,Qi Zeng,Jihui Lu,Junshuai Wang,Yongli Liu,Bing Xu,Haimin Lei
Qingfei Decoction (QFD) is recognized as one of the 100 classic prescriptions by the National Administration of Traditional Chinese Medicine of China and is widely used for the treatment of pulmonary diseases. Chronic obstructive pulmonary disease (COPD) is a common respiratory condition primarily characterized by airway obstruction. It’s necessary to examine the therapeutic effect of QFD in the treatment of COPD and elucidate its potential effective components, targets, and pathways. This study utilized UHPLC coupled with HRMS to identify the chemical constituents of QFD, resulting in the qualitative analysis of 68 compounds. Network pharmacology predicted 30 gene targets, including IL6, AKT1, and EGFR, and revealed 45 compounds, including ruscogenin, schisandrin A, and esculetin that may contribute to its therapeutic effects on COPD. Subsequently, an elastase-induced COPD mouse model was employed to evaluate the efficacy of QFD. The effects of QFD were assessed through hematoxylin and eosin (H&E) staining, periodic acid-Schiff (PAS) staining, and real-time quantitative polymerase chain reaction (RT-qPCR) on lung tissues. Transcriptomic analysis indicating QFD treatment of COPD primarily acted on the IL-17 signaling pathway, which was consistent with the network pharmacology results. Furthermore, RT-qPCR, immunofluorescence, and western blot demonstrated reduced mRNA and protein expression levels of TRAF3IP2, TRAF6, IL17, and TNFα. These findings confirmed that QFD effectively reduced inflammation, likely by down-regulating the IL-17 signaling pathway, thereby treating COPD.
研究领域:
中医药学
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药理学
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呼吸系统疾病
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分子生物学
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产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）