JOURNAL OF PROTEOME RESEARCH
·
2023
·
IF 4.4
Shaobo Yang,Hong Yang,Yanlei Huang,Gong Chen,Chun Shen,Shan Zheng
Hirschsprung’s disease (HSCR) is a congenital digestive tract malformation characterized by the absence of intramural ganglion cells in the myenteric and submucosal plexuses along variable lengths of the gastrointestinal tract. Although the improvement of surgical methods has allowed great progress in the treatment of HSCR, its incidence and postoperative prognosis are still not ideal. The pathogenesis of HSCR remains unclear to date. In this study, metabolomic profiling of HSCR serum samples was performed by an integrated analysis of gas chromatography–mass spectrometry (GC–MS) and liquid chromatography–high-resolution tandem mass spectrometry (LC–HRMS/MS) as well as multivariate statistical analyses. Based on the random forest algorithm and receiver operator characteristic analysis, 21 biomarkers related to HSCR were optimized. Several amino acid metabolism pathways were identified as important disordered pathways of HSCR, among which tryptophan metabolism was crucial. To our knowledge, this is the first serum metabolomics study focusing on HSCR, and it provides a new perspective for explaining the mechanism of HSCR.
研究领域:
医学遗传学
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代谢组学
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儿科
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DOI
PubMed
高影响因子
Bioanalysis
·
2022
·Vol. 14
·期 7
·
IF 2.695
Xueyuan Zhang,Yuhuan Ji,Jinzhi Liu,Ji Liu,Chunlei Li,Laixin Wang,Min Meng,Limei Zhao
Background: Because of the delicate nature of liposomes, bioanalysis of free and liposomal-encapsulated drugs is among the most challenging assays to perform. Current regulatory guidance for bioanalysis is not sufficient to address the complexity of this particular formulation. Method & results: Three individual LC–MS/MS methods to quantify free amphotericin B (10–3000 ng/ml) and encapsulated amphotericin B (100–50,000 ng/ml) in pretreated human plasma and total amphotericin B (100–50,000 ng/ml) in human plasma were fully validated and applied to a bioequivalence study. The acceptance criteria and experimental design of additional validation tests using cross quality control were carefully deliberated a priori and included in the sample analysis as well. Discussion: Additional validation tests are necessary to demonstrate that the measured concentration of the intended component is accurate and free of interference from other coexisting components in the sample. These practices can be used as guidance for future liposomal drug method validation.
研究领域:
药理学
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分析化学
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临床医学
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DOI
PubMed
高影响因子
SEPARATION AND PURIFICATION TECHNOLOGY
·
2024
·
IF 8.1
Jiale Lu,Amin Jv,Hongyu Zhao,Guangbo Che,Bo Feng,Yufei Zhang,Chunbo Liu,Renquan Guan
MIL-101(Cr) is an ideal material for wastewater treatment due to its large specific surface area, excellent water stability, and chemical stability. However, its limited light absorption capacity hinders its application. We loaded ferrocene carboxylic acid (Fc-COOH) onto MIL-101(Cr) by a post-synthetic modification method, which resulted in the MOF possessing excellent optical properties while maintaining its original skeleton structure. The MIL-101(Cr)/Fc-COOH (1:2), (abbreviated as CFCC-2) exhibited the best performance, achieving a removal rate of 96% for tetracycline (TC) in just 30 min. This removal rate is significantly higher compared to MIL-101(Cr) and Fc-COOH, which achieved removal rates of only 15% and 21%, respectively. We propose a possible Z-type heterojunction mechanism between MIL-101(Cr) and Fc-COOH to explain the excellent photocatalytic performance of CFCC-2. The intermediates in TC were identified using LC-MS, and the toxicity of these intermediates was predicted and evaluated through the Toxicity Estimation Software Tool (T.E.S.T.). This study provides new insights into the design and fabrication of MIL-101(Cr)-based catalysts as photodegrading organic pollutants.
研究领域:
环境科学
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材料科学
·
化学
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DOI
高影响因子
BIOCHEMICAL AND BIOPHYSICAL RESEARCH COMMUNICATIONS
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2014
·
IF 2.281
Zhengyi Chen,Yongle Li,Shuhai Lin,Meiping Wei,Fuyou Du,Guihua Ruan
In this study, an easy and efficiency protein digestion method called continuous microwave-assisted protein digestion (cMAED) with immobilized enzyme was developed and applied for proteome analysis by LC–MS n . Continuous microwave power outputting was specially designed and applied. Trypsin and bromelain were immobilized onto magnetic micropheres. To evaluate the method of cMAED, bovine serum albumin (BSA) and protein extracted from ginkgo nuts were used as model and real protein sample to verify the digestion efficiency of cMAED. Several conditions including continuous microwave power, the ratio of immobilized trypsin/BSA were optimized according to the analysis of peptide fragments by Tricine SDS–PAGE and LC–MS n . Subsequently, the ginkgo protein was digested with the protocols of cMAED, MAED and conventional heating enzymatic digestion (HED) respectively and the LC–MS n profiles of the hydrolysate was compared. Results showed that cMAED combined with immobilized enzyme was a fast and efficient digestion method for protein digestion and microwave power tentatively affected the peptide producing. The cMAED method will be expanded for large-scale preparation of bioactive peptides and peptide analysis in biological and clinical research.
研究领域:
生物化学
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蛋白质组学
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临床研究
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DOI
PubMed
高影响因子
MOLECULES
·
2026
·Vol. 31
·期 4
·721
·
IF 5.1
Juhua Zhong,Yishuo Zhu,Bin Xia,Faying Jiang,Zhengyue Qiu,Lewei Zhao,Siyu Chen,Hongbao Chen,Haobo Wang,Lin Kang,Tonghe Yang,Shuai Li,Si Liu,Jianguo Zeng,Zhixing Qing
Lilies (Liliumspp.) are highly valued in China for their edible and medicinal properties; however, bitterness in certain varieties limits consumer acceptance. Although historically attributed to colchicine, the presence of alkaloids in lilies remains a subject of debate. This research screened five lily species for colchicine and its 15 biosynthetic precursors, usingGloriosa superbaandColchicum autumnaleas positive controls. While detected in the controls, none were detected in any tissues (bulbs, roots, stems, flowers, and leaves) of the five lilies. A comparative analysis of five lily varieties—Longyahong, Lanzhou,Lilium lancifolium, Longya, and Guiyanghong—revealed that Longyahong exhibited the strongest bitterness, which was localized exclusively in the bulb peels. Based on comparative LC-MS profiling between bitter and non-bitter varieties, three high-abundance compounds were selected for isolation and subsequent sensory evaluation. Two monomeric compounds were isolated and confirmed via chromatographic methods as the primary bitter components. This study provides compelling chemical and biochemical evidence of the presence of colchicine in the examined lilies. By identifying two specific bitter components in Longyahong bulb peels, these findings refute the long-standing misconception regarding colchicine in lilies and provide a chemical foundation for improving the palatability and commercial value of bitter lily varieties.
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PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2025
·
IF 4
Lei Ding,Chundan Ye,Junchen Zhu,Cuirong Sun
Chiral impurity analysis presents significant challenges due to limitations of detection methods. Levodopa (L-Dopa) is the primary medication for Parkinson's disease treatment for over 50 years. However, the detection of its chiral impurity is difficult due to the similarity of polarity. This study presents a novel analytical method for the quantitative detection of trace amount of D-Dopa, as well as other three impurities. The method demonstrated excellent chromatographic resolution for D-Dopa and L-Dopa (resolution = 4.15) and achieved a derivatization efficiency of 97% using a chlorine-labeled chiral probe (D-BPCl) for chemical derivatization, followed by analysis with liquid chromatography-tandem mass spectrometry (LC-MS/MS) on a conventional C18 column. Meanwhile, D-BPCl showed strong chiral selectivity on D-Dopa, and the ratio of mass spectrometric response for labeled D-Dopa to that of L-enantiomers was 2.78-fold under the same condition. The developed method demonstrates high sensitivity with detection limits of 7.88 μ g L -1 for D-Dopa, and 9.85 μ g L -1 for L-Dopa, with good linearity for every analyte (R 2 > 0.99), recoveries ranging from 94.1% to 106.8%, and high repeatability with relative standard deviation (RSD) values predominantly below 5%. Then the method was applied to analyze fifteen batches of levodopa tablets from five manufacturers. D-Dopa was successfully detected with the corresponding content ranging from 0.15% to 0.44%, which suggests that D-Dopa are more likely generated during the production process. The study underscores the significant safety concerns regarding Dopa-containing medications.
研究领域:
药物分析
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药物质量控制
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手性分离
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药物代谢
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分析化学
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DOI
PubMed
高影响因子
RAPID COMMUNICATIONS IN MASS SPECTROMETRY
·
2025
·Vol. 39
·期 21
·e10117
·
IF 1.7
Dan Li,Ling Yan,Thomas Ka-Yam Lam,Zongwei Cai
Rational Investigating TCE glutathione (GSH) conjugation metabolites is essential, as these reactive intermediates play a central role in TCE bioactivation and are implicated in organ-specific toxicities, including nephrotoxicity, hepatotoxicity, and neurotoxicity. Characterizing and quantifying these metabolites enhances our understanding of TCE metabolism, supports biomarker discovery, and helps elucidate mechanisms of TCE-induced toxicity. Methods A robust liquid chromatography–tandem mass spectrometry (LC–MS/MS) method was established for the detection and quantification of three major GSH-related TCE metabolites: S-(1,2-dichlorovinyl)-glutathione (DCVG), S-(1,2-dichlorovinyl)-L-cysteine (DCVC), and N-acetyl-S-(1,2-dichlorovinyl)-L-cysteine (NAcDCVC). Serum samples were obtained from male C57BL/6 mice chronically exposed to TCE (100 ppm in drinking water for 15 weeks). Results Calibration curves for all three metabolites demonstrated excellent linearity ( R 2 > 0.998). The method achieved limits of detection (LOD) ranging from 0.0057 to 0.0120 nM, limits of quantitation (LOQ) from 0.0189 to 0.0401 nM, recoveries of 75.9%–115.5%, and inter-assay variation of 0.5%–11.5%. PD model mice exhibited elevated serum levels of DCVG and DCVC, while NAcDCVC levels were significantly reduced. Conclusion This study presents the first comprehensive LC–MS/MS-based quantification of TCE GSH conjugation metabolites in serum, offering high sensitivity, precision, and reproducibility. The observed elevated serum levels of the toxic metabolites DCVG and DCVC, along with the markedly reduced NAcDCVC concentrations in PD mice, provide a critical foundation for future investigations into the mechanistic links between TCE exposure and PD pathogenesis.
研究领域:
分析化学
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毒理学
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神经科学
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药理学
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生物化学
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DOI
PubMed
高影响因子
Foods
·
2026
·Vol. 15
·期 3
·
IF 6
Weiying Lu,Yumei Chen,Yuge Niu,Liangli (Lucy) Yu
Coffee proteins are key precursors of roasting flavor. However, heat-driven changes in the bean proteome remain underexplored. This work aimed to investigate these changes and study proteomic markers of the coffee bean. The green and roasted coffee beans were quantified for their total soluble protein and compared by sodium dodecyl sulfate–polyacrylamide gel electrophoresis (SDS–PAGE) and liquid chromatography–mass spectrometry (LC–MS) proteomics. The protein profiles identified by LC–MS were processed using principal component analysis (PCA) and partial least-squares discriminant analysis (PLS–DA) modeling to identify possible roast-sensitive protein markers. The alkaline-aided aqueous extract protein concentration was reduced from 14–23 g to 3–10 g/100 g dry weight (DW). SDS–PAGE showed dominant 17–26, 34–43, and 55–72 kDa bands weakened after roasting, while high molecular peaks (>180 kDa) were present only in roasted samples. In-solution tryptic digestion yielded nine protein groups. PCA scores revealed partial separation of green and roasted groups, while PLS-DA delivered unambiguous classification (Q2> 0.90 by cross-validation). The variable importance in projection scores highlighted that structural proteins in common plant beans are markedly down-regulated after roasting, indicating heat-induced structural disruption. The identified protein groups represent candidate markers associated with severe thermal treatment and provide possible molecular targets for investigating flavor precursor development.
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PubMed
高影响因子
CLINICA CHIMICA ACTA
·
2025
·
IF 2.9
Feng Chen,Xiaoxia Yang,Yayun Tan,Huanhuan Li,Yan Yan,Xiang Zhao,Chengfeng Qiu
Pneumocystis jirovecii pneumonia (PJP) is a high-mortality fungal infectious disease, and the changes in tryptophan metabolism and its diagnostic value in PJP remain unclear. This study aimed to elucidate the specific tryptophan metabolic profile in PJP patients by establishing and validating an LC-MS/MS method for the simultaneous quantification of tryptophan and its nine key metabolites in human serum. Serum samples from 46 PJP patients, 35 pulmonary tuberculosis (PTB) patients and 40 healthy controls were analyzed. The method achieved complete chromatographic separation within 5.5 min, with an extraction recovery rate > 95.8 % and matrix effects ranging from 86.0 % to 106.8 %, meeting the comprehensive validation criteria set by FDA and EMA guidelines. PJP patients exhibited significantly higher serum levels of 3-hydroxykynurenine (3−HK) compared to the PTB and healthy control groups (26.0 vs. 11.5 vs. 8.94 ng/mL, p < 0.001), while levels of 5-hydroxytryptophan and indole-3-acetic acid were significantly lower ( p < 0.05). The 3-Hydroxyanthranilic Acid/3-hydroxykynurenine ratio was also markedly reduced in the PJP group. ROC analysis demonstrated strong diagnostic performance for PJP with 3-hydroxykynurenine (AUC = 0.919), 5-hydroxytryptophan (AUC = 0.816), indole-3-acetic acid (AUC = 0.705), and the 3-Hydroxyanthranilic Acid/3-hydroxykynurenine ratio (AUC = 0.743). The validated LC-MS/MS method is rapid, sensitive, high-throughput and enables precise analysis of tryptophan metabolism. The distinct metabolic signature—particularly elevated 3-hydroxykynurenine, reduced 5-hydroxytryptophan and indole-3-acetic acid, and an altered 3-Hydroxyanthranilic Acid/3-hydroxykynurenine ratio—provides novel biomarkers for PJP diagnosis and offers new insights into its immunometabolic mechanisms.
研究领域:
传染病学
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代谢组学
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临床化学
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免疫代谢
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分析化学
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DOI
PubMed
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2023
·Vol. 415
·期 25
·6345-6353
·
IF 4.3
Wang Aimin,Fan Yuting,Fu Jun,Song Fengrui,Liu Zhiqiang,Liu Shu
Metabolomics is a biochemical analysis tool for identifying metabolic phenotypes and used to reveal the pathogenic mechanisms of disease and to inform drug-targeted therapies. Carboxyl-containing metabolites (CCMs) account for an important proportion of the metabolome, but because of the diversity of physical and chemical properties of CCMs in biological samples, traditional liquid chromatography–mass spectrometry (LC-MS) targeted metabolome analysis methods cannot achieve simultaneous quantification of multiple types of CCMs. Therefore, we proposed for the first time a targeted metabolomics strategy using isoniazid derivatization combined with LC-MS/MS to simultaneously quantify 39 CCMs of 5 different types (short-chain fatty acids, amino acids, bile acids, phenylalanine and tryptophan metabolic pathway acids) with large polarity differences associated with Alzheimer’s disease (AD) and significantly improve the detection coverage and sensitivity. The yields of isoniazid derivative CCMs were high and could guarantee the accuracy of CCM quantification. The LODs of CCMs increased significantly (1.25–2000-fold) after derivatization. The method showed good selectivity, intra-day and inter-day accuracies and precisions, and repeatability. There was no significant effect on the determination of CCMs in terms of matrix effect and recovery. CCMs showed good stability. And CCMs showed good stability under short-term storage and freeze-thaw cycles. At the same time, the regulatory effects of Schisandrae chinensis Fructus and Ginseng Radix et Rhizoma (SG) herb pair on CCM metabolic disorders in feces, urine, serum, and the brain of AD rats were elucidated from the perspective of targeted metabolomics. In combination with pharmacodynamic evaluation and gut microbiota analysis, the mechanism of SG herb pair on AD rats was comprehensively understood. In summary, this innovative isoniazid derivatization combined with a targeted metabolomics method has great potential for trace biological lineage analysis. Graphical
研究领域:
代谢组学
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分析化学
·
神经退行性疾病
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药理学
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中医药学
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肠道微生物
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DOI
高影响因子
CURRENT PHARMACEUTICAL BIOTECHNOLOGY
·
2021
·Vol. 22
·期 2
·274-280
·
IF 2.837
Shixing Zhu,Jiayuan Zhang,Zhihua Lv,Mingming Yu
Background: Apigenin, a natural plant flavone, has been shown to possess a variety of biological properties. Objective: In this report, a highly selective and sensitive LC-MS/MS method was developed and validated for the determination of apigenin in rat plasma. Methods: Analysts were separated on the HSS T3 column (1.8 μm 2.1×100 mm) using acetonitrile and 0.1% formic acid in 2mM ammonium acetate buffer at a supply rate of 0.200 mL/min as eluent in gradient model. Results: Plasma samples were treated by protein precipitation using acetonitrile for the recovery ranging from 86.5% to 90.1% for apigenin. The calibration curves followed linearity in the concentration range of 0.50-500ng/mL. The inter-day and intra-day precisions at different QC levels within 13.1% and the accuracies ranged from -10.6% to 8.6%. Conclusion: The assay has been successfully applied to the pharmacokinetic study of apigenin in rats.
研究领域:
分析化学
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药理学
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生物分析
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药学
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DOI
高影响因子
ANALYST
·
2020
·Vol. 146
·期 5
·1725-1733
·
IF 3.978
Chang Shu,Teng-Fei Li,Duo Li,Zhong-Qiu Li,Xing-Hua Xia
Protein drugs showing strong pharmaceutical activity, high specificity, and low toxicity and side effects have drawn extensive attention in the field of life sciences and medicine. Precise evaluation of the function of these drugs requires accurate and sensitive detection methods. Here, we report a novel chromatography-tandem mass spectrometry (LC-MS/MS) method for sensitive and selective detection of protein drugs. Magnetic nanoparticles (Apt29@MNPs) were functionalized by thrombin aptamers, and quantum dots (Apt15@ss@QDs) were dual-functionalized with quantitative thrombin aptamers and small molecules with high ionization efficiency as the mass barcode. After Apt29@MNPs specifically purify and enrich thrombin from biological samples, they can form a nano “sandwich structure” when Apt15@ss@QDs are added, resulting in the release of the mass barcode for LC-MS/MS analysis via the cutting of the disulfide bond. Since there is a higher quantitative molecular ratio of mass barcode to thrombin in the nano-“sandwich structure”, quantitative detection of thrombin with high sensitivity and selectivity can be achieved via the LC-MS/MS detection of the mass barcode with high ionization efficiency rather than thrombin, which effectively avoids the disadvantages of direct protein detection by mass spectrometry. The established method for thrombin detection shows a good linear relationship in a concentration range of 0.00115–1.15 nM with a limit of detection (LOD) of 0.0007 nM. The present work provides a new approach for the effective and sensitive quantitative analysis of protein drugs and would be of great significance in promoting the development of protein drugs and clinical applications.
研究领域:
分析化学
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生物化学
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药学
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临床医学
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DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）