JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2021
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IF 3.205
Kai Zhang,Hui Yan,Ruina Liu,Ping Xiang,Kaifei Deng,Ji Zhang,Ya Tuo,Zhenyuan Wang,Ping Huang
The determination of cause of death is one of the most important tasks in forensic practice. However, asphyxia is a difficult cause of death to determine, especially when the deceased has an underlying disease that can lead to a sudden unexpected death, such as coronary atherosclerotic heart disease (CAHD, which is the leading cause of sudden cardiac death, SCD), because its determination is currently still based on an exclusion strategy. In this study, gas chromatography coupled with high-resolution mass spectrometry (GC-HRMS)-based untargeted metabolomics was employed to obtain the pulmonary metabolic profiles of rats who died from asphyxia and SCD. First, fourteen metabolites were identified to investigate the mechanism of death from asphyxia, and we proposed some explanations that may account for these metabolic alterations, including the perturbation of amino acid metabolism, lipid metabolism, and energy metabolism (TCA cycle). Second, we discovered eight potential biomarkers to differentiate between asphyxia and SCD as the cause of death. The excellent classification performances of the eight individual biomarkers and their combination in fresh lung tissue were observed. Third, we also explored the relative change in the concentration of the eight metabolites and their classification performance in decomposed tissue (at 24 h postmortem). Lactic acid, pantothenic acid, and the combination of the eight biomarkers can be recognized as perfect classifiers to discriminate asphyxia from SCD even when decomposition has occurred. Our results showed that GC-HRMS-based untargeted metabolomics can be used as a promising tool to explore the metabolic alterations of the death process and to determine the cause of death.
研究领域:
法医学
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代谢组学
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病理学
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产品关联
DOI
PubMed
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
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2024
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IF 3.8
Huo Jinfeng,Zhe Wei,Zhang Yipeng,Yang Qianxu,Zeng Zhongda
The chemical components of natural fragrant plant extracts are of high complexity, and the strategies for quality control (QC) and further discovery of fragrance mechanisms still need to be further investigated. This study integrated the strategies and methods of untargeted metabolomics and chemometrics and statistical modeling to attain the goal. The techniques of reversed-phase and HILIC analysis of ultra-performance liquid chromatography-high-resolution mass spectrometry (UPLC-HRMS) were simultaneously used to collect data in both positive and negative ion modes. The pattern analysis of fingerprints and discovery of characteristic molecular markers for QC analysis were comprehensively employed to reach in-depth analysis of the quality variation and discovery of differential molecules among natural fragrant plant extracts. The former uses fingerprint technique to analyze their overall similarities and differences, and the latter comprehensively discovers molecular substances characterizing the chemical characteristics of fragrant extracts with the help of metabolomics and univariate and multivariate methods. The findings are expected to be used as the molecular markers in product manufacturing, sales, and consumption to achieve accurate quality control and recognition of targeted molecules for potential quality monitoring using spectroscopy techniques. In this work, 27 natural fragrant extracts were applied as examples, and their chemical components were comprehensively analyzed with discovery of markers for quality control. After data integration, 1178 molecules were annotated, and 267 differential metabolite molecules with the values of variable importance in the projection (VIP) larger than 1.0 were found. The results show that the method proposed in this work is of great significance for high-coverage analysis, QC marker discovery, and aroma mechanism elucidation, which has potential applications in the areas of food, cosmetics, pharmaceuticals, tobacco, and others. Graphical Abstract
研究领域:
分析化学
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植物学
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食品科学
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药学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2024
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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
Frontiers in Molecular Biosciences
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2021
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IF 5.246
Zhou Peipei,Zhou Lin,Shi Yingying,Li Zhuolun,Liu Liwei,Zuo Lihua,Zhang Jun,Liang Shuhong,Kang Jian,Du Shuzhang,Yang Jing,Sun Zhi,Zhang Xiaojian
The incidence of cerebral ischemic stroke characterized by high mortality is increasing every year. Danshen Chuanxiongqin Injection (DSCXQ), a traditional Chinese medicine (TCM) preparation, is often applied to treat cerebral apoplexy and its related sequelae. However, there is a lack of systematic research on how DSCXQ mediates its protective effects against cerebral ischemia stroke. Metabolomic analysis based on UHPLC-Q-Orbitrap HRMS was employed to explore the potential mechanisms of DSCXQ on ischemic stroke induced by transient middle cerebral artery occlusion (MCAO). Pattern analysis and metabolomic profiling, combined by multivariate analysis disclosed that 55 differential metabolites were identified between Sham group and Model group, involving sphingolipid metabolism, glycerophospholipid metabolism, phenylalanine, tyrosine and tryptophan biosynthesis, primary bile acid biosynthesis, pantothenate and CoA synthesis and valine, leucine and isoleucine biosynthesis pathways. DSCXQ could reverse brain metabolic deviations in stroke by significantly upregulating the levels of L-tryptophan, Lyso (18:0/0:0), LPC (18:2), Indole-3-methyl acetate, and downregulating the levels of sphinganine 1-phosphate, L-threonic acid, glutaconic acid and N6,N6,N6-Trimethyl-L-lysine. In our study, we focused on the neuroprotective effects of DSCXQ against neuroinflammatory responses and neuronal apoptosis on a stroke model based on sphingolipid metabolism. The expressions of Sphk1, S1PR1, CD62P, Bcl-2, Bax, and cleaved Caspase-3 in brain tissue were evaluated. The neurological deficit, cerebral infarct size and behavioral abnormality were estimated. Results showed that DSCXQ intervention significantly reduced cerebral infarct size, ameliorated behavioral abnormality, inhibited the expression of Sphk1, S1PR1, CD62P, Bax, Cleaved Caspase-3, while increased the level of Bcl-2, and prevented neuronal apoptosis. The limitations are that our study mainly focused on the verification of sphingolipid metabolism pathway in stroke, and while other metabolic pathways left unverified. Our study indicates that SphK1-SIP axis may potentiate neuroinflammatory responses and mediate brain damage through neuronal apoptosis, and DSCXQ could suppress the activity of SphK1-SIP axis to protect brain tissue in cerebral ischemia. In conclusion, this study facilitates our understanding of metabolic changes in ischemia stroke and the underlying mechanisms related to the clinical application of DSCXQ.
研究领域:
药理学
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神经科学
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代谢组学
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中医药
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产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
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2024
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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
ENVIRONMENTAL POLLUTION
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2025
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IF 7.3
Haixia Jin,Yong Wang,Junning Liu,Qun Gao,Jing Ji,Geyu Liang,Xiaoxia Gu,Kai Luo
Considering only parent polycyclic aromatic hydrocarbons (PAHs), such as benzo(a)pyrene as a representative compound, may underestimate the carcinogenic risk of polycyclic aromatic compounds (PACs). Nitrated polycyclic aromatic hydrocarbons (nitro-PAHs), known for their higher toxicity relative to parent PAHs, are widely present in the environment. In this study, a novel, highly sensitive, and accurate method utilizing ultra-performance liquid chromatography coupled with hybrid quadrupole Orbitrap high resolution MS (Q-Orbitrap-HRMS) was developed to quantify 15 amino-PAHs, which are metabolites of nitro-PAHs, in human urine samples. Our analysis revealed the presence of 10 out of the 15 targeted amino-PAHs in urine samples obtained from adults residing in Nanjing, China. The cumulative concentrations of the 10 amino-PAHs (∑ 10 amino-PAHs) in each urine sample ranged from not detected (ND) to 19.12 ng/mL, with mean and median concentrations of 2.85 and 2.09 ng/mL, respectively. Risk assessment using the potency equivalency factor (PEF) indicated that the mean estimated cancer risks for 1,6-dinitropyrene and 1,8-dinitropyrene, two dinitro-PAHs classified by the International Agency for Research on Cancer (IARC) as possibly carcinogenic to humans (Group 2B), were 2.96 × 10 −4 and 4.93 × 10 −5 , respectively, exceeding the commonly accepted risk threshold of 1 × 10 −6 , and indicating a potential public health concern. Overall, this study established a robust method for the identification and quantification of amino-PAHs in urine samples, highlighting the presence of nitro-PAHs, particularly dinitro-PAHs, in the human body and their significant yet often overlooked carcinogenic potential, necessitating further investigation and attention.
研究领域:
环境科学
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分析化学
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毒理学
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公共卫生
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质谱分析
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产品关联
DOI
PubMed
高影响因子
Food Chemistry-X
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2023
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IF 6.1
Jincheng Li,Ruidong Zhou,Guangxin Yang,Essy Kouadio Fodjo,Tengwang Feng,Huiwu Sun,Dongmei Huang,Cong Kong,Huan Liu
In this study, a novel filter-press cleanup column was developed as a single-step cleanup approach for the rapid screening and quantification of 112 veterinary drugs in fish samples. Fish muscle samples were extracted with acetonitrile and ethyl acetate, sequentially. After concentration and reconstitution, N -propylethylenediamine (PSA) sorbent, packed in filter-press column, allows rapid single-step cleanup operation, while UHPLC-Q-Orbitrap-HRMS provides high-precision mass information in multi-residue screening. Under optimum settings, the detection and quantification limits were validated at 0.5 and 2.0 μg·kg −1 , for all analytes, respectively. The ranges of recoveries were from 35.3 to 138.4%. Most of these target analytes (82%) could be measured with recoveries between 60 and 130%, and intra-day RSDs ranging from 1.9 to 26.1%. This method was further applied to evaluate the residual of veterinary drugs in fish samples from four cities in China, and results demonstrated its practicability for multi-residue monitoring veterinary residues for food safety administration.
研究领域:
分析化学
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食品科学
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环境科学
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产品关联
DOI
PubMed
高影响因子
Canadian Journal of Chemistry
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2024
·Vol. 102
·期 9
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IF 1.1
Bin Chen,Lirong An,Feng Li,Yanan Tang
Monitoring organic pollutants in rainwater is important to understand relations between air pollutants and water safety. Non-targeted liquid chromatography–mass spectrometry (LC–MS) is a powerful tool but because of big differences of pollutants in polarity, ionization efficiency, and low concentrations, it is challenging to detect all pollutants in a single analysis. Chemical derivatization is a widely adapted strategy to fractionate complex samples with enhanced sensitivity and selectivity. Herein, we propose the usage of dansylation as a chemical derivatization method to improve both LC retention and MS ionization of organic pollutants containing amine, hydroxyl, and carboxyl for non-targeted LC–MS analysis. We first evaluated the labeling coverage of dansylation to organic pollutants in water matrix. Using dansyl chloride (DnsCl) and dansyl hydrazine (DnsHz) to label 100 amine- and hydroxyl-containing compounds and 100 carboxyl compounds, respectively, we found DnsCl and DnsHz had over 60% labeling coverage for 8 categories of compounds. Then dansylation was applied to label the rainwater, source water, disinfected rainwater, and drinking water samples. To facilitate the annotation of dansylated compounds, we also established a web-based tool termed DansylFinder. Using DansylFinder, 3889, 5813, 6077, and 4050 tentative annotations were found in rainwater, source water, disinfected rainwater, and drinking water samples by dansylation-based non-targeted LC-HRMS analysis. Four hundred fifty four were persistently detected in all water samples, suggesting significant organic overlaps of the four water samples. In addition, two degradation pathways reported in drinking water disinfection process were also detected in disinfected rainwater, suggesting rainwater is a potential path for air pollutants to infiltrate drinking water system.
研究领域:
环境科学
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分析化学
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DOI
高影响因子
Frontiers in Pharmacology
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2020
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IF 4.225
Wang Xiao-Shuang,Sun Zhi,Liu Li-Wei,Du Qiu-Zheng,Liu Zhang-Suo,Yang Yan-Jie,Xue Peng,Zhao Hong-Yu
Background: Oral lichen planus (OLP) is a T-cell-mediated chronic inflammatory disorder and precancerous oral lesion with high incidence. The current diagnostic method of OLP is very limited and metabolomics may provide a new approach for quantitative evaluation.Methods: The Ultra-Performance Liquid Chromatography-Quadrupole/Orbitrap High Resolution Mass Spectrometry (UHPLC-Q-Orbitrap HRMS) was applied to analyze the change of metabolites in serum of patients with OLP. A total of 115 OLP patients and 124 healthy controls were assigned to either a training set (n = 160) or a test set (n = 79). The potential biomarkers and the change of serum metabolites were profiled and evaluated by multivariate analysis.Results: Totally, 23 differential metabolites were identified in the training set between OLP group and healthy group. Three prominent metabolites in receiver operating characteristic (ROC) were selected as a panel to distinguish OLP or healthy individuals in the test set, and the diagnostic accuracy was 86.1%.Conclusions: This study established a new method for the early detection of OLP by analyzing serum metabolomics using UHPLC-Q-Orbitrap HRMS, which will help in understanding the pathological processes of OLP and identifying precancerous lesions in oral cavity.
研究领域:
医学
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代谢组学
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病理学
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DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2023
·
IF 3.4
Yuzhu Chai,Erlong Zhang,Zhuoer Cai,Dan Xu,Chunxia Zhu,Baiwang Sun
Letermovir is a cytomegalovirus inhibitor for cytomegalovirus infection a hematopoietic-cell transplantation. In the degradation test of Letermovir, five new impurities were detected at levels of ND ∼ 2.21 % (by oxide, thermal or photolytic). These impurities were synthesized directly, characterized and identified by HRMS NMR spectra and X-ray crystallography. Then co-injected with commercial products to confirm their retention times in HPLC . The possible formation pathways and synthetic methods of these impurities were discussed in details. Furthermore, the toxicological properties of impurities were evaluated by ACD/Percepta 14.52.0 (Build 3525) software.
研究领域:
药学
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分析化学
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毒理学
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DOI
PubMed
高影响因子
Journal of Pharmaceutical Analysis
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2025
·
IF 8.9
Yuxuan Li,Zhenggen Piao,Songze Wang,Longhai Cui,Xinyan Li,Jinlong Ma,Chengqiang Han,Xi-Ling Li,Toufeng Jin,Jun Zhe Min
Colorectal cancer (CRC) is a prevalent gastrointestinal malignancy. However, the lack of diagnostic accuracy of traditional clinical serum biomarkers carcinoembryonic antigen (CEA) and Cancer antigen 19-9 (CA19-9) results in patients being diagnosed at an advanced stage. Herein, we developed a novel method of ultrahigh-performance liquid chromatography coupled to quadrupole-Orbitrap high-resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) for relative quantification based on the non-specific enzyme pronase E and an isotope mass spectrometry probe d0/d5-BOTC to screen novel glycan biomarkers. We applied the method in a cohort of 102 serum samples (including 51 healthy volunteers (HV), 26 stage II CRC, and 25 stage III CRC) and 90 tissue samples (including 45 paracancerous tissue and 45 cancerous tissue). Results revealed that the serum levels of H5N4F, H5N4F3SA, H4N5F1SA, and H5N4SA2 in CRC patients were significantly different from those in HV ( p < 0.01). The area under the curve values of H5N4F, H5N4F3SA, and H4N5F1SA in serum samples were 0.77, 0.71, and 0.91, respectively. The clinical diagnostic accuracies of these glycans ranged from 65% to 91%, which were significantly higher than those of CEA. Additionally, differential glycan profiles in tissues were further examined using the same method and compared with serum levels. H5N4F was found to be significantly down-regulated in all CRC groups ( p < 0.0001), indicating strong specificity for CRC diagnosis. The glycans identified in this study are expected to serve as potential biomarkers for the early diagnosis of CRC, offering valuable reference points for clinical diagnosis and treatment.
研究领域:
医学
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生物化学
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肿瘤学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2022
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IF 3.571
Baole Zhang,Wanglong Xu,Chuanlong Yin,Yangming Tang
Under the guideline issued by Food and Drug Administration (FDA), ANDAs for Certain Highly Purified Synthetic Peptide Drug Products That Refer to Listed Drugs of rDNA Origin Guidance for Industry , a synthetic Semaglutide that is intended to be a “generic” of the approved rDNA origin Semaglutide is under exploring. Thus, each peptide-related impurity that is 0.10% of the drug substance or greater need to be identified for Semaglutide covered by this guidance. Among others, characterization of the low-level D -amino acid (D form) isomeric impurities are always the most challenging ones. Reverse-phase high-performance liquid chromatography (RP-UPLC) was used to separate the impurities, followed by high resolution mass spectrometry (HRMS) to determine the molecular weight of the impurities that existed in both formulations. Following the targeted D form isomers off-line collection, the samples went through lyophilization, deuterated hydrochloric acid ( D -HCl) hydrolyzation with low level D/L form shifting suppression substrates, chiral derivatization and RP-UPLC tandem mass spectrometry analysis of different amino acids by comparing with standards. Herein, we reported an accurate, straightforward characterization method with low limit of detection for the low-level D -Ser 8 , D -His 1 and D -Asp 9 Semaglutide impurities in Semaglutide formulations. The developed UPLC tandem HRMS method entails a valuable step forward in the detection of trace levels of the D -isomers of Semaglutide and other peptide products.
研究领域:
药学
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分析化学
✓ 已验证
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）