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BIOMEDICAL CHROMATOGRAPHY · 2017 ·Vol. 32 ·期 4 ·e4156 · IF 1.613

Simultaneous determination of tryptophan, kynurenine, kynurenic acid, xanthurenic acid and 5-hydroxytryptamine in human plasma by LC-MS/MS and its application to acute myocardial infarction monitoring

Qing Tong,Jia Song,Guangjie Yang,Li Fan,Wei Xiong,Jianguo Fang

Reliable methods for the determination of tryptophan and its metabolites are vital to the monitoring of biochemical states during the initiation and progression of cardiovascular disease. In the present study, a single-run liquid chromatography–tandem mass spectrometry (LC-MS/MS) method was developed for the simultaneous determination of tryptophan (Trp) and its metabolites, including kynurenine (Kyn), kynurenic acid (KA), xanthurenic acid (XA) and 5-hydroxytryptamine (5-HT), in human plasma. The plasma samples were prepared using a protein precipitation approach, and the chromatographic separation was performed by gradient elution on a C 18 column within a total analysis time of 3.5 min. The calibration ranges were 40–20,000 ng/mL for Trp, 4–2000 ng/mL for Kyn, 0.2–100 ng/mL for KA, 0.4–200 ng/mL for XA and 1–500 ng/mL for 5-HT, and the precision and accuracy were acceptable. The evaluation of recovery and internal standard-normalized matrix effect proved that the sample preparation approach was effective and the matrix effect could be negligible. The newly developed method was successfully applied to the analysis of plasma samples from healthy individuals and myocardial infarction patients. The findings suggested that the plasma concentrations of Trp, Kyn, 5-HT as well as the concentration ratios of Kyn/Trp and Trp/5-HT might serve as biomarkers for the monitoring of acute myocardial infarction.

研究领域: 临床化学 · 心血管疾病 · 分析化学
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BIOMEDICAL CHROMATOGRAPHY · 2015 ·Vol. 30 ·期 3 ·426-431 · IF 1.723

Pharmacokinetic study of ofloxacin enantiomers in Pagrosomus major by chiral HPLC

Jing Nie,Yang–Guang Wang,Xiao–Feng Gao,Xiao–kun OuYang,Li–Ye Yang,Di Yu,Wei–jian Wu,Hong–Ping Xu

( S )-(−)-Ofloxacin and ( R )-(+)-ofloxacin concentrations in the plasma of Pagrosomus major after drug treatment were detected by chiral high-performance liquid chromatography, and various pharmacokinetic parameters were calculated from these data. The elimination half-life of ( S )-(−)-ofloxacin was significantly shorter than that of the ( R )-(+) enantiomer. ( S )-(−)-Ofloxacin also had a significantly lower maximum plasma concentration, area under the concentration–time curve from zero to infinity, and mean residence time than ( R )-(+)-ofloxacin. However, the apparent volume of distribution and total body clearance of ( S )-(−)-ofloxacin were greater than those of ( R )-(+)-ofloxacin. The ratio of the ( S )-(−)- to ( R )-(+)-ofloxacin plasma concentration was always <1.0. Together, these data suggest that ( S )-(−)-ofloxacin was preferentially excreted and ( R )-(+)-ofloxacin was preferentially absorbed. Although the difference in pharmacokinetic parameters was small, the metabolic behavior of the ofloxacin enantiomers in P. major was enantioselective. Copyright © 2015 John Wiley & Sons, Ltd.

研究领域: 药理学 · 分析化学 · 海洋生物学
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BIOMEDICAL CHROMATOGRAPHY · 2026 ·Vol. 40 ·期 7 ·e70494 · IF 1.7

Discovery of Q-Markers of Mudan Granules by Chemical Profile, Pharmacokinetics, Neuroprotective Effect Evaluation, and Network Pharmacology

Zhiyan Wang,Shiqi Zhang,Chenxiu Hu,Shufang Wang

Mudan granules (MDs) are a widely used Chinese patent medicine for treating diabetic peripheral neuropathy (DPN). TCM quality is the basis to ensure its efficacy; however, the current quality standard for MD relies on the control of only two constituents derived from the minister drugs. Therefore, it is necessary to establish a more comprehensive quality evaluation system based on rational quality markers (Q-markers). In this study, Q-markers of MD were discovered through systematic evaluations. Thirty-seven compounds were newly characterized in MD by UPLC-QTOF-MS. Among all the 173 constituents in MD, 64 were found to be absorbed into the bloodstream and/or sciatic nerve of rats in prototype. The contents of 24 candidate Q-markers were determined, and the pharmacokinetics features of nine ones were analyzed by two developed UPLC-MS methods. Six candidate Q-markers were first found to exhibit protective effects on Schwann cells against the injury of high glucose/lipid. Finally, nine Q-markers were screened, and network pharmacology analysis showed that the enriched pathways for these nine Q-markers covered the major DPN-related pathways for the full set of 173 constituents. The results provide important evidence for improving the quality control system of MD and reference for discovering Q-markers of other TCM prescriptions.

✓ 已验证 DOI PubMed 高影响因子
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BIOMEDICAL CHROMATOGRAPHY · 2024 ·Vol. 38 ·期 6 ·e5866 · IF 1.8

A fast and efficient liquid chromatography–tandem mass spectrometry method for measuring l- and d-amino acids in the urine of patients with immunoglobulin A nephropathy

Zhijian Zha,Ruihua Wang,Qian Wang,Fahui Chen,Ziyang Ye,Yafeng Li

Immunoglobulin nephropathy (IgAN) stands as the most prevalent primary glomerular nephropathy globally, typically diagnosed through an invasive renal biopsy. Emerging research suggests the significant involvement of chiral amino acids in kidney disease progression. This study introduces a nonderivative LC–tandem mass spectrometry approach, offering efficient separation outcomes within 15 min for identifying chiral amino acids in human urine samples. Subsequently, using this method, the analysis of l - and d -amino acids in the urine of both patients with IgAN and healthy individuals was conducted. Fourteen d -amino acids and 20 l -amino acids were identified in the urine samples obtained from 17 patients with IgAN and 21 healthy individuals. The results indicated notable variances in the concentrations of both l - and d -amino acids between the IgAN and healthy control groups. In contrast to the healthy group, the IgAN group exhibited higher mean urine concentrations of most l -amino acids and lower concentrations of d -amino acids. Furthermore, correlations between amino acids and clinical markers were investigated. These results propose a novel method for monitoring trace amino acids in urine samples and introduce a new concept for potential markers of IgAN.

研究领域: 医学 · 分析化学 · 肾脏病学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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BIOMEDICAL CHROMATOGRAPHY · 2019 ·Vol. 34 ·期 2 ·e4727 · IF 1.748

Anti-hyperuricemia activity and toxicity prediction of a novel xanthine oxidoreductase inhibitor

Liping Zhou,Baxiong Wei,Lvying Wu,Jing Li,Bin Zhu,Lei Zhang

A potent xanthine oxidoreductase inhibitor (LS087) was recently proved to exhibit a similar hypouricemic potency to febuxostat. A hyperuricemia model induced by potassium oxonate and hypoxanthine was proposed in specific pathogen-free male Kunming mice, and the serum urea nitrogen, creatinine and uric acid levels were measured after oral administration of LS087. Furthermore, renal histopathology was conducted by staining with hematoxylin and eosin, periodic acid–Schiff and Masson's trichrome stains, respectively. The results showed that the levels of serum urea nitrogen and uric acid significantly decreased compared with the model group, but the level of creatinine showed no significant changes. The pathological abnormalities in kidney tubules were improved after LS087 administration. Ten metabolites (M1–M10) of LS087 were identified after a single oral dosing of 10 mg/kg in rats. M6 was the primary LS087 metabolite in vivo with a pathway of methylation. The toxicity and potential risks of LS087 and its metabolites were predicted using the ProTox-II software. LS087 and the major metabolites (M2, M3, M5, M6, M7 and M8) were predicted to have no potential hepatotoxicity, but some metabolites with a total rate of <1% (M1, M4, M9, and M10) showed potential hepatotoxicity. M1 and M8 showed potential carcinogenicity. The LS087 biotransformation pathway in rat was well characterized.

CAS / MDL: 9004-32-4 9085-26-1
✓ 已验证 产品关联 DOI PubMed 高影响因子
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BIOMEDICAL CHROMATOGRAPHY · 2012 ·Vol. 27 ·期 4 ·509-514 · IF 1.966

Identification of isoquercitrin metabolites produced by human intestinal bacteria using UPLC-Q-TOF/MS

Linling Lu,Dawei Qian,Jing Yang,Shu Jiang,Jianming Guo,Er-xin Shang,Jin-ao Duan

In this paper, ultraperformance liquid chromatography/quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF/MS) and the MetaboLynx™ software combined with mass defect filtering were applied to identity the metabolites of isoquercitrin using an intestinal mixture of bacteria and 96 isolated strains from human feces. The human incubated samples collected for 72 h in the anaerobic incubator and extracted with ethyl acetate were analyzed by UPLC-Q-TOF/MS within 10 min. The parent compound and five metabolites were identified by eight isolated strains, including Bacillus sp. 17, Veillonella sp. 23 and 32 and Bacteroides sp. 40, 41, 56, 75 and 88 in vitro . The results indicate that quercetin, acetylated isoquercitrin, dehydroxylated isoquercitrin, hydroxylated quercetin and hydroxymethylated quercetin are the major metabolites of isoquercitrin. Furthermore, a possible metabolic pathway for the biotransformation of isoquercitrin was established in intestinal flora. This study will be helpful for understanding the metabolic route of isoquercitrin and the role of different intestinal bacteria in the metabolism of natural compounds. Copyright © 2012 John Wiley & Sons, Ltd.

CAS / MDL: 482-35-9
研究领域: 分析化学 · 微生物学 · 代谢组学
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BIOMEDICAL CHROMATOGRAPHY · 2025 ·Vol. 39 ·期 2 ·e6067 · IF 1.7

Evaluation of the Impact of HIFU on Peptide Bond Formation: A Study Using SPE-LC-MS/MS Methodology

Jiale Liu,Rongfei Yuan,Qi Wang,Hai Qiao,Yuling Yang,Siyu Yang,Hua Zhang,Chang Chen

High-intensity focused ultrasound (HIFU) is a noninvasive soft tissue ablation technique, which utilizes ultrasound energy to induce thermal coagulation necrosis in targeted tissues. Whether this high energy causes side effects in vivo, such as the formation of peptide bonds, has not been fully investigated. Glycylglycine is the simplest dipeptide and hence is often used as a model compound for peptide studies. In this study, we developed and validated a sensitive quantification method based on ion-exchange solid-phase extraction, liquid chromatography, and tandem mass spectrometry (SPE-LC-MS/MS) for the analysis of glycylglycine without derivatization, and then used it to evaluate whether HIFU promoted peptide bond formation in aqueous solution (without enzymes) and plasma (with enzymes). The results showed that strong cation exchange SPE significantly reduced the matrix effect and improved the sensitivity of the LC-MS/MS method. No formation of glycylglycine in the aqueous solution or plasma was observed following HIFU irradiation.

CAS / MDL: 14091-11-3 103616-89-3
研究领域: 生物化学 · 医学工程
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BIOMEDICAL CHROMATOGRAPHY · 2023 ·Vol. 38 ·期 1 ·e5772 · IF 1.8

Simple and rapid determination of triclabendazole and its metabolites in bovine and goat muscle tissue

Feng Xu,Ting Yang,Jiayong Yu,Yinliang Wu

Triclabendazole (TCB) is widely used for prevention and treatment of parasitic infections in animals. Improper use can result in drug residues in animal tissues and cause health problems to humans through consumption. A simple and reliable analytical method for the determination of TCB and its metabolites in bovine and goat muscle using liquid chromatography–tandem mass spectrometry (LC–MS/MS) was developed and validated. Analytes were extracted using acetonitrile and purified using enhanced matrix removal cartridge. Chromatographic separation was carried out on a BEH Shield RP18 column. The analytes were detected in positive-mode electrospray ionization mass spectrometry using multiple reaction monitoring. Average recoveries of 96.1%–105.6% with coefficients of variation of 1.9%–8.4% were obtained at fortification levels of 0.5, 2.5, 25, and 50 μg/kg for TCB and 5.0, 25, 250, and 500 μg/kg for its metabolites (triclabendazole sulfoxide, triclabendazole sulfone, and keto-TCB). A good linear regression was obtained with the mixed standard solutions in the range of 0.05–20 μg/L for TCB and 0.5–200 μg/L for its metabolites. The limit of quantification and limit of detection ranged from 0.05 to 0.75 μg/kg and from 0.1 to 1.5 μg/kg, respectively. Moreover, this method was successfully applied to 33 real samples.

CAS / MDL: 64-18-6
✓ 已验证 产品关联 DOI PubMed 高影响因子
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BIOMEDICAL CHROMATOGRAPHY · 2023 ·Vol. 37 ·期 12 ·e5743 · IF 1.8

Development of a joint derivatization protocol for the unequivocal identification of the monosaccharide composition in four dendrobium polysaccharides and free monosaccharide by GC–MS

Wei-Han Yang,Jing-Wen Hao,Nai-Dong Chen,Jiao Li

The determination of monosaccharides is crucial for studying the structure of polysaccharides and the composition of free monosaccharides in living organisms. Based on previous derivatization gas chromatography–mass spectrometry (GC–MS) methods, we aimed to develop a novel analytical protocol for better quantifying monosaccharides. In this study, sugar alcohol acetylation, saccharonitrile acetylation, silylation and a combination of sugar alcohols acetylation and saccharonitrile acetylation were compared. The optimal method was verified with the monosaccharide determination of four polysaccharides and four free monosaccharides from Dendrobium . The results showed that the novel combined derivatization method was superior to the other three methods in terms of content analysis of monosaccharides. Furthermore, it possessed good linearity (all calibration curves showed relative coefficients ≥ 0.999), sensitivity, precision (relative standard deviation < 2%), and accuracy (recovery, 95.7–105%). Finally, the novel method established in this study was successfully employed in determining the monosaccharide composition of four polysaccharides and four free monosaccharide samples from Dendrobium .

CAS / MDL: 50-99-7 87-89-8
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BIOMEDICAL CHROMATOGRAPHY · 2023 ·Vol. 37 ·期 11 ·e5732 · IF 1.8

Integrated network pharmacology and metabolomics analyses of the mechanism underlying the efficacy of Ma-Mu-Ran Antidiarrheal Capsules against dextran sulfate sodium–induced ulcerative colitis

Hailing Huang,Bailu Duan,Sili Zheng,Yan Ye,Dongning Zhang,Zhuang Huang,Shanshan Wang,Fengyun Zhang,Ping Huang,Fang Huang,Lintao Han

The current study utilizes a comprehensive network pharmacology and metabolomics analysis to investigate the mechanism of action of Ma-Mu-Ran Antidiarrheal Capsules (MMRAC) for the treatment of ulcerative colitis (UC). In this study, we established a mouse model of UC using dextran sulfate sodium. Colonic tissues were collected from mice and then subjected to hematoxylin and eosin staining, as well as histopathological analysis, to assess the therapeutic effect of MMRAC. Furthermore, we assessed the mechanisms through which MMRAC combats UC by employing integrated metabolomics and network pharmacology strategies. Lastly, we validated the key targets identified through western blot and molecular docking. An integrated network of metabolomics and network pharmacology was constructed using Cytoscape to identify eight endogenous metabolites involved in the therapeutic action of MMRAC on UC. Further comprehensive analyses were focused on four key targets and their associated core metabolites and pathways. The results of western blot and molecular docking demonstrated that MMRAC could modulate key targets and their expression levels. The cumulative results indicated that MMRAC restored intestinal function in UC, reduced inflammatory responses, and alleviated oxidative stress by influencing the methionine and cysteine metabolic pathways, as well as the urea cycle. In addition, it had an impact on arginine, proline, glutamate, aspartate, and asparagine metabolic pathways and their associated targets.

✓ 已验证 产品关联 DOI PubMed 高影响因子
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BIOMEDICAL CHROMATOGRAPHY · 2023 ·Vol. 37 ·期 12 ·e5751 · IF 1.8

Improved LC–MS/MS method for the simultaneous quantification of tacrolimus and cyclosporine A in human blood and application to therapeutic drug monitoring

Feng Chen,Xiaoxia Yang,Huanhuan Li,Xiaodan Zeng,Ziwei Deng,Hongqiang Wang,Yuanxiang Jin,Chengfeng Qiu,Zhihua Shi

In order to facilitate therapeutic drug monitoring of tacrolimus and cyclosporine A in clinical practice, a simple, rapid, robust, sensitive and specific LC–MS/MS assay was developed and validated for the simultaneous determination of tacrolimus and cyclosporine A in human whole blood. Erythrocytes were destroyed using internal standard solution with 10% (w/v) zinc sulfate in water. The analytes were extracted from 100 μl of whole blood by protein precipitation with acetonitrile. Chromatographic separation was conducted on a Kinetex PFP column (60°C) by a gradient elution with a flow rate of 0.450 ml/min in 2.5 min. Quantitative analysis was performed using electrospray ionization and multiple reaction monitoring in positive ionization mode. The method was fully validated as per current guidelines on bioanalytical methodologies of the US Food and Drug Administration and European Medicines Agency. The method developed was applied successfully in analyzing clinical samples from patients administered tacrolimus or cyclosporine A. The sample treatment procedure was rationalized and improved to fulfill the complete target extraction. The chromatography conditions were optimized to achieve rapid and accurate quantification of both analytes. This method may be beneficial as a constructive input for the therapeutic drug monitoring of tacrolimus and cyclosporine A in obtaining individualized therapy.

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BIOMEDICAL CHROMATOGRAPHY · 2014 ·Vol. 28 ·期 12 ·1738-1743 · IF 1.662

Bioavailability comparison of a new form of vilazodone XVII to IV in beagles using liquid chromatography/mass spectrometry

Ling-ling Zeng,Li-li Sun,Qiaogen Zou,Fan Zhou,Ping Wei,Ping-kai Ouyang

Vilazodone hydrochloride (CAS 163521-12-8) is polymorphic and has 15 crystal forms, referred to as I–XI and XIII–XVI. In the study, we prepared and performed structural identification of a new crystal form named XVII. To investigate this in vivo , a rapid and sensitive method based on liquid–liquid extraction, followed by high-performance liquid chromatography–tandem mass spectrometry (HPLC-MS/MS) was developed and validated for the determination of vilazodone hydrochloride in dog plasma. This HPLC-MS/MS method was successfully applied to a bioavailability comparison of two crystal forms of vilazodone hydrochloride (IV and XVII) in six healthy beagles using a single-dose, two-way crossover design. The maximum plasma concentration ( C max ), the time taken to reach C max , and the area under the concentration–time curve were determined following oral administration of 10 mg vilazodone hydrochloride (IV or XVII) to beagles. These analyses revealed no significant bioavailability differences between vilazodone hydrochloride forms IV and XVII in dogs. Copyright © 2014 John Wiley & Sons, Ltd.

CAS / MDL: 631-61-8
研究领域: 药学 · 分析化学
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