Scientific Reports
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2017
·Vol. 7
·期 1
·1-15
·
IF 4.259
Sun Zhi,Zuo Lihua,Sun Tongwen,Tang Jinfa,Ding Daling,Zhou Lin,Kang Jian,Zhang Xiaojian
To clarify and quantify the chemical profiling of XueBiJing injection (XBJ) rapidly, a feasible and accurate strategy was developed by applying ultra high performance liquid chromatography-Q Exactive hybrid quadrupole-orbitrap high resolution accurate mass spectrometry (UHPLC-Q-Orbitrap HRMS). A total of 162 components were characterized, including 19 phenanthrenequinones, 33 lactones, 28 flavonoids and 12 phenolic acids and 51 other compounds. Among them, 38 major compounds were unambiguously quantified by comparing with reference standards. Meanwhile, 38 representative compounds were simultaneously detected in XBJ samples by Q-Orbitrap HRMS. Satisfactory linearity and correlation coefficient were achieved with wide linear range. The precisions, repeatability, stability and recovery were meeting requirements. The validated method was successfully applied for simultaneous determination of 38 bioactive compounds in 10 batches XBJ samples. In addition, the similarity evaluation of fingerprintings was applied to assess the quality of XBJ. And the results were evaluated by multiple statistical strategies and five compounds might be the most important chemical markers for chemical quality control of XBJ. Finally, a rapid and simple UPLC-MS/MS method was developed for determination of five markers in XBJ sample. This research established a high sensitive and efficient strategy for integrating quality control, including identification and quantification of XBJ.
研究领域:
药学
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分析化学
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DOI
PubMed
高影响因子
TALANTA
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2025
·
IF 6.1
Ruiquan Ding,Mengdie Li,Yawen Zhang,Hongyi Liu,Zhenyu Tang,Xiyue Xiong,Yingzhuang Chen,Ming Ma,Bo Chen
The selective analysis of isoprene-containing natural products, such as triterpenoid saponins and prenylated flavonoids, remains a major challenge in analytical chemistry due to their substantial structural diversity and poor ionization efficiency, which hampers their detection in complex matrices like herbal extracts. To address this pressing need, we developed an analytical platform that integrates the Paternò-Büchi (PB) reaction with LC-HRMS, employing 4,4'-dichlorobenzophenone as the derivatization agent. High selectivity was achieved through a novel dual-filtering strategy combining a characteristic neutral loss (Δm/z = 276.03) with a distinctive chlorine isotope signature (M+2:M+3≈9:6). This approach significantly enhanced detection sensitivity for model compounds (up to 3.8-fold) and reduced false-positive signals in complex herbal extracts by up to 79%. The method was successfully validated using Panax notoginseng and Epimedium extracts, enabling the tentative identification of 42 isoprene-containing natural products, including 29 triterpenoid saponins and 13 flavonoids. In addition, the stereoselectivity of the PB reaction provided structural insight into local steric hindrance, critical for analyzing isomeric saponins, and the platform demonstrated excellent reproducibility, with relative standard deviations (RSDs) below 5.0%. This study presents a robust and highly selective platform for functional group-specific analysis, offering a powerful new tool for natural product research. By significantly enhancing the accuracy and efficiency of isoprenoid screening, it facilitates the discovery of bioactive compounds and holds promise for broad applications in metabolomics, herbal medicine quality control, and the discovery of novel drug leads from natural sources.
研究领域:
分析化学
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天然产物化学
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代谢组学
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植物化学
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质谱分析
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PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2021
·
IF 4.759
Shuping Hu,Min Zhao,Zhongle Wang,Jiaying Yang,Dawei Chen,Pengcheng Yan
A simple extraction procedure coupled with liquid chromatography-Q Orbitrap high resolution mass spectrometry (LC-Q Orbitrap HRMS) for the determination of 19 quinolones in animal-derived foods (pork, fish, egg and milk) has been developed. Sample preparation is based on homogeneous liquid-liquid extraction at pH > 9 using water-miscible acetonitrile with cold-induced phase separation. The procedure allowed one-step enrichment and cleanup of all the 19 quinolones with different logP properties to lower aqueous phase, which eliminated the process of preconcentration and re-dissolution for sample solution. Furthermore, an adsorption phenomenon was observed between conventional borosilicate glass injection vials and most of quinolones. In detection analysis, a scheduled variable full scan strategy was performed to improve detection performance in Q Orbitrap HRMS. Under optimal conditions, a superior limit of quantitation (0.028–0.192 μg/kg) in animal-derived foods was achieved using this proposed method. Lastly, this method was validated and applied successfully in real samples.
研究领域:
分析化学
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食品安全
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DOI
PubMed
高影响因子
CARBOHYDRATE POLYMERS
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2025
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IF 12.5
Qing-Hua Liu,Liu Yang,Yue Wang,Hao-Ming Xiong,Cai-Yun Wang,Guo-Yuan Zhu,Li-ping Bai,Zhi-Hong Jiang,Wei Zhang
Polygonatum odoratum ( P. odoratum ) oligosaccharides (POO) are bioactive compounds with complex structures. Since the precise structure of POO remains undefined, their pharmacological development and clinical application have been hindered. This study developed a universal strategy to elucidate oligosaccharide structures of P. odoratum by combining Orbitrap high-resolution mass spectrometry (Orbitrap-HRMS) and enzymatic hydrolysis. Initially, monosaccharide constituents of free oligosaccharides (POO) and polysaccharides (POP) in P. odoratum were quantitatively analyzed. The accurate mass values, retention time, and sequence-specific fragment information facilitated initial characterization by comparing with the self-established oligosaccharide library based on these monosaccharides. Due to the limitations of MS in precisely identifying isomer structures, enzymatic hydrolysis was further employed to distinguish the glycosidic linkage and oligosaccharide type. Fructanase mixture, endo -1,4-β-mannanase, exo -1,3-β-D-glucanase, α-galactosidase and amyloglucosidase were used to identify hexose-based isomers, while α-L-arabinofuranosidase and endo -1,4-β-xylanase were used for pentose-based isomers. The study revealed that POO primarily consisted of fructooligosaccharides, and its isomers, such as 1-kestose, 6-kestose, and neokestose, were clarified. POP mainly comprised galactomannan, with the branching site at α-(1 → 6)-galactoside in POPO determined for the first time in P. odoratum . This strategy provides a straightforward methodology for analyzing plant oligosaccharides, establishing a structure analytical foundation for further pharmacological research and potential clinical applications.
研究领域:
植物学
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天然产物化学
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分析化学
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糖生物学
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植物化学
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PubMed
高影响因子
ANALYTICAL CHEMISTRY
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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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高影响因子
Frontiers in Pharmacology
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2018
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IF 3.831
Zuo Lihua,Zhou Lin,Xu Tanye,Li Zhuolun,Liu Liwei,Shi Yingying,Kang Jian,Gao Guanmin,Du Shuzhang,Sun Zhi,Zhang Xiaojian
Xuebijing (XBJ) injection is an ethnomedicinal formula that has been widely used in the therapy of sepsis in China. However, the underlying theraputic mechanisms remain uninvestigated. In this research, a metabolomic method based on UHPLC-Q-Orbitrap HRMS was applied to make a holistic evaluation of XBJ on septic rats which were induced by the classical cecal ligation and puncture (CLP) operation. The plasma metabolic changes were profiled and evaluated by multivariate analytical (MVA) methods. In the results, a total of 41 differential metabolites were identified between CLP-operated group and sham-operated group, which were mainly involved in amino acid metabolism and lipid metabolism. After pathway analysis, it was finally discovered that the majority of the influenced metabolic pathways caused by sepsis mainly involved in energy metabolism, oxidative stress, and inflammation metabolism. When intervened by XBJ injection, 32 of the 41 disordered metabolites had been adjusted in reverse, which suggested that XBJ could mediate the abnormal metabolic pathways synergistically. In conclusion, the present study systematically investigated the efficacy and its underlying therapeutic mechanisms of XBJ on sepsis, while offering a new insight for the subsequent relevant exploration of other Chinese medicine at the same time.
研究领域:
药理学
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代谢组学
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中医药学
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PubMed
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
Analytical Methods
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2026
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IF 3
Yiming Tian,Yixin Gu,Jianfeng Wu,Jia Chen,Jinqiao Jiang,Yulong Liu,Wei You,Kaikai Li,Jianwei Xie
Synthesis route attribution enables accurate source tracing of chemical warfare agents and effective discrimination between distinct synthetic pathways. In the current study, we report for the first time the identification of trace process-related impurities derived from the synthesis of the vesicant ethyl sesquimustard, which is listed in Schedule 1.A.04 of the Chemical Weapons Convention (CWC). Using 1,2-ethanedithiol and 2-mercaptoethanol as precursors, 22 different synthetic routes were designed, and 88 batches of samples were produced through micro-synthesis. Gas chromatography-high resolution mass spectrometry (GC-HRMS) coupled with a non-targeted screening strategy was employed to analyze route-specific compounds. The obtained dataset was further used to train the orthogonal partial least squares discriminant analysis algorithm and generate a classification model consisting of eight sub-models. The verification results showed that the overall classification accuracy of the model was 21/22 (about 95%).
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DOI
PubMed
高影响因子
Drug Testing and Analysis
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2026
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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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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
ANALYTICAL CHEMISTRY
·
2021
·
IF 6.986
Caiming Tang,Jianhua Tan,Caixing Tang,Deyun Liu,Peilin Zhang,Xianzhi Peng
Distributions of chlorine isotopologues are potentially a fingerprint feature of organochlorines. However, the exact distributions remain little known. This study measured compound-specific chlorine isotopologue distributions of six polychlorinated organic compounds (POCs) for source identification. Complete chlorine isotopologues of POCs were detected by gas chromatography coupled to high-resolution mass spectrometry. The measured relative abundances (Ameas), theoretical relative abundances (Atheo), and relative variations between Ameas and Atheo (ΔA) of chlorine isotopologues were determined. These ΔA values were applied to characterize differences in isotopologue distribution patterns, and the ΔA patterns directly illustrated the distribution characteristics. Perchloroethylene (PCE) and trichloroethylene (TCE) from two manufacturers were chosen as model analytes to develop and validate the analytical method, including precision, concentration dependency, and temporal drift. The ΔA values of isotopologues of the PCE and TCE chemicals were from −82.5 to 19.9‰ with standard deviations (SDs) of 0.3–16.9‰. In addition, the ΔA values of the first three isotopologues (with 0–2 37Cl atoms) were from −15.5 to 19.9‰ with SDs of 0.3–1.6‰, showing sufficient precisions. No concentration dependency and temporal drift of ΔA were observed. The method has been successfully applied to source identification for PCE and TCE in commercial chemicals and plastic materials, and four polychlorinated biphenyls in chemicals and sediments, demonstrating that the ΔA values and ΔA patterns were discernable for POCs from different sources. This study demonstrates that compound-specific chlorine isotopologue distributions of POCs are differentiable and measurable, proposing a novel approach to perform fingerprinting analysis for the distributions, which is anticipated to facilitate source identification for organochlorine pollutants.
研究领域:
环境科学
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分析化学
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PubMed
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
·
生物化学
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PubMed
高影响因子
危险品化学品经营许可证（带存储）