MICROCHIMICA ACTA
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2018
·Vol. 185
·期 6
·1-10
·
IF 5.705
Yang Wen,Li Tengfei,Shu Chang,Ji Shunli,Wang Lei,Wang Yan,Li Duo,Mtalimanja Michael,Sun Luning,Ding Li
A method is described for the determination of proteins with LC-MS/MS enabled by a small molecule (adenosine) barcode and based on a double-recognition sandwich structure. The coagulation protein thrombin was chosen as the model analyte. Magnetic nanoparticles were functionalized with aptamer29 (MNP/apt29) and used to capture thrombin from the samples. MNP/apt29 forms a sandwich with functionalized gold nanoparticles modified with (a) aptamer15 acting as thrombin-recognizing element and (b) a large number of adenosine as mass barcodes. The sandwich formed (MNP/apt29-thrombin-apt15/AuNP/adenosine) can ben magnetically separated from the sample. Mass barcodes are subsequently released from the sandwiched structure for further analysis by adding 11-mercaptoundecanoic acid. Adenosine is then detected by LC-MS/MS as it reflects the level of thrombin with impressively amplified signal. Numerous adenosines introduced into the sandwich proportional to the target concentration further amplify the signal. Under optimized conditions, the response is linearly proportional to the thrombin concentration in the range of 0.02 nM to 10 nM, with a detection limit of 9 fM. The application of this method to the determination of thrombin in spiked plasma samples gave recoveries that ranged from 92.3% to 104.7%.
Schematic representation of a method for the determination of thrombin with LC-MS/MS. The method is based on a double-recognition sandwiched structure. With LC-MS/MS, mass barcodes (adenosine) are detected to quantify thrombin, which amplifies the detection signal impressively.
研究领域:
分析化学
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蛋白质组学
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医学检测
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FOOD CHEMISTRY
·
2026
·
IF 9.8
Jia-bo Huang,Yi-hui Tang,Jing Li,Jing-ru Chen,Peng-fei Jiang
Non-targeted metabolomics was employed to investigate key metabolites and metabolic pathways influencing sea urchin quality during frozen storage (−18 °C) under different packaging methods (normal, nitrogen, and vacuum). Comparative analysis revealed significant metabolic variations between frozen and fresh samples. KEGG enrichment analyses demonstrated that the metabolism of the normal packages was more disturbed, while there was a significant accumulation of polyunsaturated fatty acids (linolenic and α-Linolenic acid). Nitrogen packaging partially mitigated oxidation, but polyunsaturated fatty acids (linolenic and eicosapentaenoic acids (EPA)) still accumulated. Vacuum packaging had the best metabolic stability, minimal changes in amino acid metabolism, and effectively inhibited the production of polyunsaturated fatty acids, thereby substantially reducing off-flavor formation. This study provides a crucial theoretical foundation for controlling quality deterioration in frozen-stored sea urchins and offers valuable insights for optimizing commercial transportation and marketing strategies.
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ANALYTICA CHIMICA ACTA
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2026
·
IF 6.1
Yue-qiang Chen,Xiao-xia Dong,Li Liu,Xiu-ping Chen,Chen-guo Feng,Li-xing Zhan,Yue Su,Fang Zhang,Yin-long Guo
Background Alterations in the amine submetabolome are closely associated with cellular metabolic status and are important for understanding metabolic regulation under intervention conditions. In this study, a stable isotope labeling derivatization combined with liquid chromatography–mass spectrometry (LC–MS) was employed to characterize alterations in the cellular amine submetabolome. Optimization of chromatographic separation and cellular metabolic quenching procedures improved the separation performance of amine metabolites while enabling more accurate preservation of the metabolic state at the time of sampling. Results The established method was applied to a D-lactate–treated BEAS-2B cell model to evaluate amine submetabolome alterations under different compound intervention conditions. The results demonstrated that selenomethionine (SeMet) and berberine alleviated D-lactate induced abnormalities in the amine submetabolome and showed metabolic regulatory effects consistent with tumor-suppressive trends observed under in vivo experiments. Significance Overall, this analytical strategy enables characterization of the amine submetabolome in complex biological samples and provides a reliable methodological reference for metabolome-based investigations of cellular metabolic alterations.
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Results in Chemistry
·
2026
·
IF 5.8
Xiaozheng Huang,Ruizi Qing,Yuqing Sun,Yuanqing Wei,Rui Liu,Shuying Han,Yuhao Teng
Accurate absolute quantification of peptides in complex matrices using LC-MS/MS is often hindered by significant matrix effects, especially in the quantitative determination of gelatin peptides in food. This study developed a strategy to reduce matrix interference in LC-MS/MS quantification of gelatin peptides by screening a simulated matrix based on physicochemical similarity. Deer antler gelatin was hydrolyzed with eight proteases and comprehensively characterized. Multivariate analyses (PCA and HCA) identified the Compound proteinase hydrolysate as most closely resembling the Trypsin-digested matrix with minimal interference, and was selected for method development. The validated method for five characteristic peptides showed excellent linearity (12.5–500 ng/mL, r 2 > 0.998), with LOQs of 0.12–5.20 ng/mL, precision RSDs of 4.45–12.44%, and accuracy of 79.5–116.9%. It was successfully applied to quantify peptides in Cervidae antler gelatin, thereby providing a practical approach to improving reliability in food quality control.
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RSC Advances
·
2025
·Vol. 15
·期 21
·16973-16982
·
IF 4.6
Haijun Wang,Qiao Zhang,Xiaolin Li,Huan Chen,Xiaolan Zhu,Liming Yang,Hongling Yin,Jing Sun,Shuhong Fang,Hui Zhang
A large-volume direct-injection (LVDI) method was developed and validated for the simultaneous analysis of 69 antibiotics in bottled water using ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Target antibiotics included 23 sulfonamides, 19 quinolones, 12 macrolides, 11 β-lactams, and 4 tetracyclines. Optimization of ion source parameters led to enhanced signal intensities for 55 antibiotics. The 100 μL injection volume was both feasible and preferred, resulting in increased signal intensities while maintaining unchanged peak shapes for the antibiotics. Good absolute recoveries for the 69 antibiotics were obtained with the LVDI method, primarily ranging from 80% to 120%, whereas lower absolute recoveries of macrolides, quinolones, sulfonamides and β-lactams were observed with a solid-phase extraction (SPE) method. The limits of detection (LODs) for antibiotics were generally comparable between the LVDI and SPE methods, with values below 1 ng L−1 for most antibiotics (0.00271–26.6 ng L−1). Analysis of 25 brands of bottled water using the LVDI method revealed the presence of 54 antibiotics from 5 classes, with detection frequencies (DFs) ranging from 4% to 100% and detected concentrations between 0.0453 and 37.4 ng L−1. Multiple antibiotics were detected simultaneously in bottled water, with more than 10 antibiotics identified in each of 9 different brands. Quinolones and sulfonamides were the predominant antibiotics, accounting for over 80% of the total concentration. Only sulfaclozine showed significantly different concentrations between purified drinking water and natural mineral water (22.2 vs. 17.2 ng L−1, p < 0.05).
研究领域:
分析化学
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环境科学
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食品科学
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TALANTA
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2025
·
IF 6.1
Keke Yi,Wei Wan,Ziyu Qu,Di Zhang,Zihong Ye,Xinhua Dai,Jie Xie,You Jiang,Xiang Fang
A determination method using a home-built quadrupole-linear ion trap tandem mass spectrometry (Q-LIT) multistage fragmentation function to accurate measure ultra-trace steroid hormones in human serum was established. The capability of ion trap for multistage fragmentation (MS 3 ) overcomes the limitation of triple quadrupole systems restricted to MS 2 , enabling deeper structural characterization. Multistage fragmentation (MS3) enables the accurate detection of steroid hormones in serum samples without requiring extensive derivatization or time-consuming sample preparation and improves sensitivity by effectively reducing noise. Hydrocortisone, 4-androstenedione, 11-deoxycortisol, 21-deoxycortisol, and 17α-hydroxyprogesterone were quantified by MS 3 transitions m/z 363.2 → 327.2→309.2, m/z 287.2 → 97.0→79.0, m/z 347.1 → 311.2→293.2, m/z 347.0 → 311.1→293.1, and m/z 331.2 → 313.3→295.2, respectively. Multistage fragmentation mass spectrometry effectively prevents matrix interference, and the quantitative results of MS 3 are less affected by matrix effect than those of MS 2 . The established multistage fragmentation quantitative method showed good linearity (R 2 ≥ 0.99), and the limits of detection and quantification of 5 steroid hormones were lower than 0.06 and 0.20 ng/mL, respectively. The recovery was 86.56 %–123.14 %, with an RSD of ≤13.57 %. A total of 22 real serum samples were accurately and sensitively measured using the Q-LIT multistage fragmentation method. Therefore, Q-LIT based multistage fragmentation has great potential for applications, such as detecting steroid hormones with severe matrix effects and distinguishing among related isomers in complex biological samples.
研究领域:
分析化学
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内分泌学
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临床医学
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2025
·
IF 3.1
Yu Qin,Shenping Zhang,Jingwen Shi,Heng Gong
Antibiotics are a class of compounds that are effective against bacterial infections and are widely used in aquaculture. Herein, a method based on high performance liquid chromatography coupled with tandem mass spectrometry was developed to detect nine classes of 116 antibiotics in aquatic products. The antibiotics were extracted in two steps using 1% formic acid-acetonitrile with 0.1 mol/L Na 2 EDTA-Mcllvain buffer solution and acetonitrile, purified using Captiva EMR-Lipid, and separated with an ACQUITY UPLC®HSS T 3 column (100 mm×2.1 mm, 3.5 μm) using acetonitrile and 0.1% formic acid with 5 mM ammonium acetate as mobile phase for gradient elution. Calibration curve from 0.10 to 100 ng/mL exhibited good correlation coefficient (R 2 >0.99) for quantification. The analytical performance of the developed method was satisfactory, with limits of quantification ≤ 5.00 ng/g for detecting of antibiotics in aquatic products. The recoveries of the 116 antibiotics ranged from 60.57% to 127.33%, with precision (expressed as relative standard deviation) of < 30.20%. All parameters showed acceptable values and conformed to the Commission Decision 2021/808/EC criteria. When compared with other techniques, the developed method meets the quantitative requirements of high-throughput analysis and can simultaneously analyze 116 antibiotics in aquatic products.
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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药理学
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JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
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2025
·
IF 6.2
Xin-Ze Wu,Kai-Wen Tan,Xu Zhang,Jun-Jie Tan,Na An,Fang Cong,Wenbin Wu,Azamat Temerdashev,Quan-Fei Zhu,Hong Wang,Yu-Qi Feng
Fatty acid esters of hydroxy fatty acids (FAHFAs) are emerging bioactive lipids in edible oils, but their trace-level presence and matrix complexity hinder accurate analysis. Here, we designed a novel chemoselective probe piperazine-modified silica (SiO2-PP) that specifically captures FAHFAs while removing almost totally triglycerides in a one-step labeling reaction. The probe enabled single-batch sample pretreatment within 30 min, integrating capture, purification, and signal amplification. Coupled with liquid chromatography–mass spectrometry, the method achieved high sensitivity (LOD: 0.0039–0.033 ng/mL) and enabled quantification of 47 FAHFA isomers in 47 vegetable oil samples, with concentrations ranging from 0.56 to 1.76 × 104 ng/g. Five dominant isomers (e.g., 10-OAHSA) were identified, with olive and peanut oils exhibiting the highest FAHFA concentrations. This approach provides a promising platform for high-throughput functional lipid profiling, effectively overcoming the inefficiencies of traditional methods while significantly enhancing the assessment of vegetable oil quality.
研究领域:
分析化学
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脂质组学
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食品科学
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生物活性脂质
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质谱分析
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Frontiers in Plant Science
·
2024
·
IF 4.1
Qian Huimin,Hu Yan,Zhang Haiwen,Chu Shanshan,Peng Huasheng
Gardeniae Fructus (Zhizi) serves as both a medicinal and edible substance and finds widespread use in various industries. There are often two kinds of medicinal materials in the market: Zhizi and Shuizhizi. Typically, Zhizi with small, round fruit is used for medicinal purposes, while Shuizhizi, characterized by large, elongated fruit, is employed for dyeing. Market surveys have revealed a diverse range of Zhizi types, and modern research indicates that Shuizhizi contains rich chemical components and pharmacological activities. In this study, we collected 25 batches of Zhizi and Shuizhizi samples, categorizing them based on appearance into obovate and round fruits, with seven length grades (A–G). Using the ultra-high performance liquid chromatography coupled with triple quadrupole mass spectrometry (UHPLC-QQQ-MS/MS) method, we simultaneously quantified 13 main chemical components in fruits of Gardenia species. In addition, we compared the weight percentage of the pericarp, flesh, and seeds parts of samples with different traits, and quantified 13 chemical components in different parts. Results indicated that, aside from a few instances of overlapping fruit size ranges, Shuizhizi generally exhibits larger and longer dimensions than Zhizi. The weight proportion of the Shuizhizi pericarp is often higher than that of the Zhizi pericarp. Quantitative results highlighted significant differences in the chemical component content between Zhizi and Shuizhizi, with Shuizhizi generally containing higher levels of iridoids. The PCA and OPLS-DA analysis distinctly divided Shuizhizi and Zhizi, among which three iridoids, two organic acids, and one flavonoid made significant contributions to their classification. Cluster heatmap analysis also demonstrated complete separation between Zhizi and Shuizhizi, with clear distinctions among Zhizi samples from different origins. The distribution of the 13 chemical components in different Zhizi and Shuizhizi parts remained consistent, with iridoids and pigments concentrated in the seeds and flesh, and two organic acids and one flavonoid enriched in the pericarp. In summary, this study contributes valuable insights for classifying Zhizi and offers guidance on the rational use of Shuizhizi and the different parts of Zhizi.
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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植物学
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MOLECULES
·
2024
·Vol. 29
·期 13
·3133
·
IF 4.2
Qimei Wu,Jinfen Zheng,Yan Yu,Zhirong Li,Ying Li,Chengfeng Hu,Yaping Zhou,Rongxiang Chen
Vitex negundohas strong antioxidant activity, but its primary antioxidant components are not clear. In this study, the antioxidant components were screened by offline two-dimensional liquid chromatography coupled with electrochemical detection (2D-LC-ECD) and subsequently assessed using liquid chromatography-tandem mass spectrometry (LC-MS/MS) identification, radical scavenging capacity, and molecular docking. Various fractions were isolated fromVitex negundoleaves, and 39 antioxidant components were screened and identified. All of the fractions containing the antioxidant components exhibited certain antioxidant activity. Correlation analysis revealed a strong correlation between the response of LC-ECD and the in vitro antioxidant activity of the fractions. Molecular docking demonstrated that components with high response to LC-ECD exhibited robust interaction with antioxidant-related target proteins. The main antioxidant components ofVitex negundoleaves were isoorientin, chlorogenic acid, agnuside, cynaroside, and scutellarin. The 2D-LC-ECD combined with LC-MS/MS was rapid and effective in screening the antioxidant components inVitex negundoleaves and could also provide technical support for the discovery of antioxidant components with different polarities and contents in other medicinal and edible plants.
研究领域:
植物化学
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分析化学
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药理学
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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
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毒理学
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法医学
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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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危险品化学品经营许可证（带存储）