INTERNATIONAL JOURNAL OF LEGAL MEDICINE
·
2024
·Vol. 138
·期 4
·1323-1328
·
IF 2.2
Yu Zhonghao,Zhao Erjuan,Shi Qing,Yuan Yuhao,Ma Jinghong,Zhou Luwang,Duan Yijie,Zhou Yiwu
Brodifacoum exerts its antagonistic effect against the metabolism of vitamin K, an essential component in the synthesis of blood coagulation factors. This effect ultimately hinders the blood’s capacity to clot effectively, rendering it a commonly employed rodenticide. Instances of lethal poisonings are exceedingly rare owing to expeditious medical intervention and treatment. Within this report, we present a case of brodifacoum-induced homicide, wherein the patient exhibited distinct clinical examinations and symptoms. Moreover, the patient’s blood sample exhibited a noteworthy brodifacoum concentration of 0.681 µg/mL even after a period of 43 days following the incident of poisoning. Although an autopsy was not conducted due to religious restrictions, we endeavor to reasonably deduce the cause of death and furnish corroborative evidence for clinical diagnosis, treatment, and forensic examination in instances involving brodifacoum poisoning.
研究领域:
医学
·
毒理学
·
法医学
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PubMed
高影响因子
Clinical Proteomics
·
2022
·Vol. 19
·期 1
·1-14
·
IF 5
Zhang Di,Li Yaohan,Liang Mingzhu,Liang Yan,Tian Jingkui,He Qiang,Yang Bingxian,Jin Juan,Zhu Wei
Background Immunoglobulin A nephropathy (IgAN), a globally common primary chronic glomerulopathy, is one of the leading causes of end-stage renal disease. However, the underlying mechanisms of IgAN have yet to be demonstrated. There were no adequate and reliable plasma biomarkers for clinical diagnosis, especially at the early stage. In the present study, integrative proteomics and metabolomics were aimed at exploring the mechanism of IgAN and identifying potential biomarkers.Methods Plasma from IgAN and healthy individuals were collected and analyzed in a randomized controlled manner. Data-independent acquisition quantification proteomics and mass spectrometry based untargeted metabolomics techniques were used to profile the differentially expressed proteins (DEPs) and differentially abundant metabolites (DAMs) between two groups and identify potential biomarkers for IgAN from health at the early stage. Disease-related pathways were screened out by clustering and function enrichment analyses of DEPs and DAMs. And the potential biomarkers for IgAN were identified through the machine learning approach. Additionally, an independent cohort was used to validate the priority candidates by enzyme-linked immunosorbent assay (ELISA).Results Proteomic and metabolomic analyses of IgAN plasma showed that the complement and the immune system were activated, while the energy and amino acid metabolism were disordered in the IgAN patients. PRKAR2A, IL6ST, SOS1, and palmitoleic acid have been identified as potential biomarkers. Based on the AUC value for the training and test sets, the classification performance was 0.994 and 0.977, respectively. The AUC of the external validation of the four biomarkers was 0.91.Conclusion In this study, we combined proteomics and metabolomics techniques to analyze the plasma of IgAN patients and healthy individuals, constructing a biomarker panel, which could provide new insights and provide potential novel molecular diagnoses for IgAN.
研究领域:
肾病学
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蛋白质组学
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代谢组学
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生物标志物发现
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系统生物学
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机器学习
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ANALYTICA CHIMICA ACTA
·
2021
·
IF 6.558
Wei Li,Pei Zhang,Xiaoying Hou,Tian Tang,Siqi Li,Ruiqi Sun,Zunjian Zhang,Fengguo Xu
Modified metabolites play significant roles in disease occurrence, progression and diagnosis. Sensitive and accurate analytical methods for the quantification of these metabolites are therefore of great importance. In this study, a liquid chromatography tandem mass spectrometry (LC-MS/MS) method was developed for the simultaneous measurement of 13 pairs of prototypes and their modified forms covering nucleobases , nucleosides and amino acids . In order to improve the quantification sensitivity and accuracy, two structure analogs named N -dimethyl-amino naphthalene-1-sulfonyl chloride (Dns-Cl) and N -diethyl-amino naphthalene-1-sulfonyl chloride (Dens-Cl) were introduced for twins labeling derivatization . Dns-labeling was utilized to react with target analytes while the Dens-labeling of standard compounds provided one-to-one internal standards. With the introduce of naphthalene and easily ionizable moiety tertiary ammonium, chromatography retention and separation of these polar metabolites were notably improved on C18 columns and the detection sensitivity was increased up to 400 folds. The method is sensitive with the lower limit of quantification (LLOQ) values of 0.002–0.5 μg/mL. Comparisons of the performance of twins labeling derivatization and traditional chemical isotope labeling (CIL) derivatization verified the ability of our method in the absolute quantification. The established method was applied to human lung adenocarcinoma cell line A549 and its cisplatin resistant derivative A549/DDP. Significant shifts in 12 metabolites as well as 9 modified-to-prototypical ratios in A549/DDP were observed, demonstrating the utility of our method and the potential role of modified metabolites in mediating anticancer drug resistance. The method can be easily extended to determine other types of modified metabolites in various biological matrices, which will greatly expand our knowledge on these metabolites.
研究领域:
分析化学
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生物化学
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药理学
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癌症研究
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代谢组学
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PubMed
高影响因子
MOLECULES
·
2020
·Vol. 25
·期 4
·839
·
IF 3.267
Yueqing Xu,Liangxiao Zhang,Ruinan Yang,Xu Yu,Li Yu,Fei Ma,Hui Li,Xiupin Wang,Peiwu Li
Vitamin K1is one of the important hydrophobic vitamins in fat-containing foods. Traditionally, lipase is employed in the determination of vitamin K1to remove the lipids, which makes the detection complex, time-consuming, and insensitive. In this study, the determination of vitamin K1in fat-containing foods was developed based on ultrasound-assisted extraction (UAE), solid-phase extraction (SPE) combined with liquid chromatography–tandem mass spectrometry (LC-MS/MS). The optimal conditions for extraction of vitamin K1were material–liquid ratio of 1:70 (g/mL), extraction temperature of 50 °C, extraction power of 700 W, extraction time of 50 min, material-wash fluid ratio of 1:60 (g/mL), and 8 mL of hexane/anhydrous ether (97:3,v/v) as the elution solvent. Then, vitamin K1was analyzed on a ZORBAX SB-C18 column (50 mm × 2.1 mm, 1.8 μm) by gradient elution with water (0.01% formic acid) and methanol (0.01 formic acid + 2.5 mmol/L ammonium formate) as the mobile phase. The limit of detection (LOD) and limit of quantification (LOQ) were 0.05 and 0.16 μg/kg, respectively. Calibration curve was linear over the range of 10–500 ng/mL (R2> 0.9988). The recoveries at three spiked levels were between 80.9% and 119.1%. The validation and application indicated that the proposed method was simple and sensitive in determination of vitamin K1in fat-containing foods.Keywords:ultrasound-assisted extraction;solid-phase extraction;LC-MS/MS;vitamin K1;foods
研究领域:
分析化学
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营养学
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高影响因子
ENVIRONMENTAL SCIENCE AND POLLUTION RESEARCH
·
2016
·Vol. 23
·期 9
·8500-8507
·
IF 2.76
Wang Dezhen,Zhang Ping,Wang Xinru,Wang Yao,Zhou Zhiqiang,Zhu Wentao
In the present study, both untargeted and targeted metabolomics approaches were used to evaluate the subacute effects of hexabromocyclododecane (HBCD) on mice urine metabolome. Untargeted metabolomics based on 1 H NMR showed that HBCD exposure disturbed mice metabolism in both dosed groups, especially in high dosed group. The low-dose HBCD led to a decrease in alanine, malonic acid, and trimethylamine (TMA). High-dose HBCD-treated mice developed high levels of citric acid and 2-ketoglutarate, together with decreased alanine, acetate, formate, TMA, 3-hydroxybutyrate, and malonic acid. Targeted metabolomics for metabolic profiling of 20 amino acids identified alanine, lysine, and phenylalanine as significantly disturbed metabolites. These results indicated that subchronic exposure to HBCD caused a disturbance of mice metabolism, especially in TCA cycle, lipid metabolism, gut microbial metabolism, and homeostasis of amino acids, and the application of untargeted and targeted metabolomics combined with conventional toxicology approaches to evaluate the subacute effects of pollutants will provide more comprehensive information and aid in predicting health risk of these pollutants.
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MICROCHEMICAL JOURNAL
·
2023
·
IF 4.8
Shu Wang,Bingliang Zhang
Nitrilotriacetic acid (NTA) and ethylenediaminetetraacetic acid (EDTA), as widely used chelating agents, have created many environmental issues and raised much attention regarding their environmental occurrence. However, the determination of NTA and EDTA in samples of complex solution chemistry remains challenging. Here, we proposed a simple and sensitive method based on liquid chromatography tandem mass spectrometry (LC-MS/MS) to determine NTA and EDTA from aqueous samples without an enrichment step. During the analysis, H + -cation exchange was used to efficiently eliminate interference from metal ions. The intensity of NTA and EDTA with trimethylsilyldiazomethane methylation could be improved hundreds of times that of the virgin samples. To maximize sensitivity, the sample pretreatment methods, the derivatization procedures and the LC-MS/MS conditions were systematically optimized. The validated method showed low limits of quantification (0.4 μg/L for NTA and 1.5 μg/L for EDTA), a wide linear response (up to several mg/L, R 2 > 0.998), and good intra- and inter-day precision (relative standard deviation ≤ 11%). The reliability of this method was successfully validated by analysis of authentic water samples collected from three WWTPs and one river with satisfactory recoveries (80–117%). It can be proposed as a powerful analytical method of NTA and EDTA in authentic water samples and could potentially be adapted to detect other chelates and polydentate compounds.
研究领域:
环境科学
·
分析化学
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BMC Chemistry
·
2023
·Vol. 17
·期 1
·1-10
·
IF 4.6
Xu Daokun,Huang Haolun,Hu Wenyan,Liu Xinmei,Yang Jun
A liquid chromatography–tandem mass spectrometry (LC–MS/MS) method was developed for the analysis of ribavirin in chicken. Samples was extracted with 0.1% formic acid and purified by Hypercarb cartridge prior to LC–MS/MS analysis. The eluates were evaporated to dryness, reconstituted in 1 mL 5mM ammonium acetate containing 5% acetonitrile (v/v) and 0.1% (v/v) formic acid. Chromatographic separation was performed on a Hypercarb analytical column under a gradient elution program with acetonitrile and 0.1% (v/v) formic acid in 5 mM ammonium acetate at a flow rate of 0.6 ml/min. The intraday and interday accuracy ranged from − 7.83 − 1.39%, and − 6.38 − 2.25%, with precisions between 1.34 − 3.88%% and 1.10 − 4.67%. The limits of detection (LODs) and limits of quantitation (LOQs) of ribavirin was 0.1 ng/mL and 0.5 ng/mL, respectively. The method was validated for linearity, accuracy, precision, matrix effect and stability. Application of the method confirmed 3 ribavirin positive samples out of 50 commercial chicken samples, with concentrations of ribavirin ranging from 0.9 μg/kg to 5.8 μg/kg a, respectively. Additionally, both AB Sciex 5500 and Agilent 6945B were proven to be suitable in ribavirin separation and quantification. The described method is suitable for the determination of ribavirin in chicken in analytical practice to monitor illegal addition of this kind of anti–viral drug.
研究领域:
分析化学
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兽药残留检测
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食品科学
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PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2024
·
IF 3.8
Lei Zhang,Xu Liu,Tenghui Jin,Jing Dong,Xiaodong Li,Youyi Zhang,Dongyang Liu
Some bile acids (BAs) were considered as biomarkers or have therapeutical effect on metabolic diseases. However, due to the existence of isomers and limitations in sensitivity, simultaneous quantification of multiple BAs remains a challenge. The aim of this study is to establish an accurate and sensitive method for the determination of multiple BAs with similar polarity. A LC-MS/MS analytical method capable of quantifying forty-five BAs simultaneously using nine stable isotope internal standards was developed and fully validated based on key isomers-oriented separation strategy. The method was further applied to analyze plasma samples to describe the dynamic profile of BAs after high glucose intake. The chromatography and mass spectrum conditions were optimized to enable the accurate quantification of forty-five BAs, while ensuring the lower limit of quantification between 0.05–10 ng/mL. The results of system suitability, linearity, dilution integrity, accuracy and precision demonstrated the good quantitative capacity and robustness of the method. A total of thirty-five BAs were quantified in plasma samples from twelve healthy Chinese individuals. The established method featured superior sensitivity and better separation efficiency compared to previous studies. Meanwhile, BAs exhibited correlations with glucose and insulin, suggesting their potential as biomarkers for metabolic disorders.
研究领域:
分析化学
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生物化学
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代谢组学
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临床化学
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高影响因子
SCIENCE OF THE TOTAL ENVIRONMENT
·
2023
·
IF 9.8
Yuling Zhong,Chenzhi Hou,Xinyi Gao,Mingyu Wang,Yan Yao,Mengyi Chen,Bin Di,Mengxiang Su
The illegal use of beta-agonists could cause severe problems to human health. In this study, the usage of beta-agonists in 31 cities across China was estimated using wastewater-based epidemiology (WBE). The proposed method is based on solid-phase extraction (SPE) and LC-MS/MS and was developed and validated to determine the concentration of seven beta-agonists in wastewater. A population model based on cotinine (COT), NH 4 -N and the flow volume was constructed to estimate the population equivalents for different wastewater treatment plants (WWTPs). Clenbuterol and ractopamine are banned in China for both animal husbandry and medical use, but were nevertheless detected in some wastewater samples at rates of 6.2 % and 4.7 %, respectively ( n = 339). The WBE-based consumption of clenbuterol and ractopamine were compared with the acceptable daily intake (ADI) and the health risks were assessed by their hazard quotients (0.26–6.62 for clenbuterol and 9.27 × 10 −4 -0.05 for ractopamine). Salbutamol, clorprenaline and terbutaline were observed in practically all wastewater samples at concentrations of up to several ng/L, whereas the formoterol and bambuterol concentrations were below the detection limit in all samples. Salbutamol consumption (7.35 ± 4.14 mg/1000 inh/day) was highest among the examined beta-agonists and varied regionally. Beta-agonist consumption based on WBE was higher in some cities than that based on medical survey data, indicating potential illegal use. These results show that WBE can be a straightforward and supplementary method for monitoring beta-agonist usage at the population level and spatially.
研究领域:
环境科学
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流行病学
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公共卫生
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分析化学
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DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2026
·
IF 4
Chenyue Zhu,Chuanxiang Yao,Huiting Qin,Wei Zhang,Xinyue Zheng,Siying Zheng,Xinyuan Ye,Ying Xiong,Lili Jiang,Sen Li,Meiqin Wang,Hongliang Jiang,Zhifeng Du
The presence of deamination impurities in phosphorothioate oligonucleotides (PS-ONs) presents a significant challenge to quality control, as their detection is complicated by minimal mass differences from the parent molecule and difficulties in chromatographic separation. Herein, a bottom-up strategy based on enzymatic digestion, chemical derivatization, and liquid chromatography-tandem mass spectrometry (LC-MS/MS) was proposed for the sensitive qualitative and quantitative analysis of trace cytosine deamination in PS-ONs. Fomivirsen (FMVS) and its deamination impurity were used as models. The method involved digestion with S1 nuclease, followed by derivatization of the 5’-phosphorothioate in digests with N-(tert-butyldimethylsilyl)-N-methyltrifluoroacetamide (MTBSTFA) to enhance chromatographic retention and mass spectrometric response. This approach effectively eliminated the need for ion-pairing (IP) reagents. The mass shift upon deamination was amplified in the smaller digested fragments, and a unique isotopic pattern in the derivatized products, specifically, the decrease of the first isotopic peak and the increase of the second isotopic peak was exploited for quantification. The method demonstrated excellent linearity over a weight ratio of deamination product to prototype range from 0.05:1 to 0.9:1. Satisfactory accuracy (80–120%) and precision (RSD < 15%) were achieved. Furthermore, the precise deamination site (C8) within a sample containing 10% deamination impurities was successfully identified. Thus, this method provides a powerful tool for profiling deamination impurities in PS-ONs, with potential applications in quality control, stability studies, and the characterization of other nucleic acid modifications.
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EUROPEAN JOURNAL OF LIPID SCIENCE AND TECHNOLOGY
·
2026
·Vol. 128
·期 9
·e70142
·
IF 2.4
Yunping Yao,Zehui Zhang,Bingxin Li,Changmo Li
Accurate qualitative and quantitative determination of free radicals during lipid oxidation, which is the core process of edible oil quality deterioration and essentially a free radical chain reaction, is of crucial importance. To overcome this problem, we developed and validated an analytical method for the specific characterization of key radicals in lipid oxidation. These radicals (R•, RO•, and ROO•) were trapped using N-tert -butyl-α-phenylnitrone under iron-mediated conditions, leading to the formation of stable adducts that were subsequently analyzed by LC–MS/MS–IT–TOF. This method offers good sensitivity with low limits of detection (0.06–0.15 µM) and limits of quantification (0.20–0.50 µM). Density functional theory calculations further confirm that the reaction proceeds readily and yields thermodynamically stable products. When applied to the methyl linoleate oxidation system, the method demonstrated that methyl linoleate alkyl radical (L•) predominated during oxidation, with its concentration peaking at 3.74 × 10 −2 mM (accounting for up to 70% of radicals) at 4 h followed by a decline due to chain termination reactions, whereas methyl linoleate peroxyl radicals (LOO•) concentration stabilized as oxidation progressed (1.46 × 10 −2 mM, 27% of radicals), and methyl linoleate alkoxyl radicals (LO•) remained at a consistently low concentration (1.58 × 10 −3 mM) owing to its preferential conversion via the β-scission pathway. These results were consistent with electron spin resonance (ESR) data, thereby validating the method's reliability. Consequently, this method enables the precise monitoring of lipid oxidation processes, serving as a valuable tool for assessing antioxidant efficacy in lipid science. Practical Applications : We present an analytical method integrating N-tert -butyl-α-phenylnitrone (PBN)-based spin trapping with LC–MS/MS–IT–TOF for direct tracking of key lipid radicals (L•, LO•, and LOO•) throughout the lipid oxidation process. This method addresses a long-standing technical gap in lipid oxidation research, providing a robust, practical tool for both high-throughput screening of high-efficacy antioxidants and rational design of stable lipid-containing food formulations. By bridging fundamental analysis and product development, our technique has clear real-world implications for extending the shelf life of lipid-based foods, offering significant value to food chemistry research while delivering substantial economic and sustainability benefits to the global food industry.
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SAUDI PHARMACEUTICAL JOURNAL
·
2025
·Vol. 33
·期 5
·1-17
·
IF 3.4
Wang Ziheng,Xu Yuchen,Liu Manting,Yang Yuchang,Shi Wenjuan,Zhu Qian,Liu Juan,Yi Lisha,Wu Huimin,Yin Xingbin,Dong Xiaoxv,Ni Jian,Qu Changhai
This study aimed to establish a method for quantifying baicalin (BC) in rabbit ocular tissues and plasma, and evaluate the pharmacological efficacy and pharmacokinetic properties of BC and BC@HS15/DSPE-PEG2000-L-Val, a novel ocular formulation for dry eye treatment. BC@HS15/DSPE-PEG2000-L-Val or free BC was administered via eye drops to benzalkonium chloride (BAC)-induced dry eye mice. Corneal and conjunctival tissues were assessed for anti-dry eye efficacy. BC concentrations in cornea, conjunctiva, aqueous humor, and ocular plasma were quantified using LC–MS/MS. Noncompartmental pharmacokinetic parameters (AUC, Tmax) were calculated using DAS 2.0 software. The method demonstrated excellent linearity (0.50–500.00 ng/mL, r > 0.9905), precision (RSD < 10%), and accuracy (± 13%). Compared to free BC, BC@HS15/DSPE-PEG2000-L-Val significantly increased tear secretion, reduced MMP-3/MMP-9 expression, and preserved corneal epithelium integrity. In the micelle group, corneal and conjunctival Cmax values were 2.7- and 3.6-fold higher than the solution group, respectively. A sensitive and validated liquid chromatography-tandem mass spectrometry (LC–MS/MS) method was developed to measure baicalin concentrations in ocular plasma and tissues of rabbits. BC@HS15/DSPE-PEG2000-L-Val for treating dry eye demonstrated significantly superior outcomes. The nano-micelle notably enhanced BC concentration on the ocular surface and effectively prolonged its retention time. Graphical abstract
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危险品化学品经营许可证（带存储）