MICROCHEMICAL JOURNAL
·
2025
·
IF 5.1
Mengmeng Feng,Huifang Ge,Ting Zhang,Jingbo Liu,Boqun Liu,Yali Yu
The quantification and analysis of free amino acids (FAAs) in serum is important for illness diagnosis due to its content varies with the body’s condition. In this study, a new sensitive analytical method based on liquid chromatography electrospray ionization mass spectrometry (LC-ESI-MS/MS) was optimized for simple and rapid simultaneous detection of 20 amino acids by pre-column derivatization. Amino acid derivatized by 9-fluorenyl methyl chloroformate (FMOC-Cl) were eluted and separated by simple mobile phase reagent in 20 min via gradient elution using a traditional reverse phase C18 column (150 × 4.6 mm, 5 μm), at the flow rate of 0.8 mL/min. After optimizing derivatization, LC-MS/MS conditions, and sample pre-treatment, this method was verified with LODs and LOQs ranging from 0.0237 to 0.2391 ng/mL and 0.079 to 0.7971 ng/mL. The intra- and inter-day precision was no more than 10 %. The overall accuracy and recovery varied from 88.4-111 % and 88.7–114 %, respectively. Those methods were first applied to mice serum with ulcerative colitis. The results showed that the levels of Ala, Arg, Trp, Lys, Cys, Tyr, and Phe significantly increased in pre-treated group by egg white peptides, which will participate in metabolism. This study provides a valuable reference for further research on the pathogenesis of ulcerous colitis and the development of functional foods to relieve inflammation and balance metabolism.
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CHEMISTRY & BIODIVERSITY
·
2025
·
IF 2.5
Tingli Qu,Shasha Suo,Liqiu Yan,Liwei Wang,Taigang Liang
Astragaloside IV (ATS) is an active component of Astragalus membranaceus, which has immune regulation and anti-inflammatory effects. However, owing to its large molecular weight and poor solubility in water, the therapeutic effects of ATS are limited. We aimed to prepare astragaloside IV-chitosan (ATS-CS) nanoparticles and determine their anti-inflammatory effect and mechanism of action on RAW264.7 cells using metabolomics. The size of the ATS-CS nanoparticles was 200.3 nm with a zeta potential of 30.5 mV, and the encapsulation rate and drug loading were 69% and 13%, respectively. ATS-CS nanoparticles not only significantly decreased the increase of NO, IL-6 and TNF-α levels induced by LPS, but also exerted an anti-inflammatory effect by acting on arginine and proline, glutathione, sphingolipid, glycerophospholipid, and glycine, serine, and threonine metabolism. Our findings confirmed that ATS-CS nanoparticles have good anti-inflammatory activity and showed that the activity of high molecular weight can be increased by producing nanoparticles. Our study paves the way for exploring the mechanism of nanoparticles through metabolomics.
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高影响因子
MOLECULES
·
2024
·Vol. 29
·期 5
·1037
·
IF 4.2
Yujie Zhang,Jingjie Cao,Jiahan Su,Tingting He,Qianru Wang,Feng Wei,Xin Guo,Qibing Mei,Jing Zeng
Bitespiramycin, has been shown to have a therapeutic effect against respiratory tract inflammation, including a potential effect against COVID-19. A current clinical trial in China showed that bitespiramycin was an effective treatment for severe pneumonia and intracranial infection. However, there is lack of an analytical method to elucidate the distribution of bitespiramycin. In this study, a highly sensitive, rapid and reliable UPLC–MS/MS method was developed to comprehensively characterize the bitespiramycin distribution in various bio-samples, which is significantly improved upon the published work. A rapid sample preparation method was developed by usingn-butanol as the solvent to extract bitespiramycin from different bio-samples. The extract was then directly analyzed by UPLC–MS/MS coupled with an alkaline-resistant column after centrifugation which avoids the time-consuming concentration process under nitrogen and redissolution. The method was employed to accurately quantify bitespiramycin and its metabolites in rat plasma, tissues, and human cerebrospinal fluid. Notably, the presence of bitespiramycin and its metabolites was identified for the first time in various rat organs including brain, testis, bladder and prostate as well as in human cerebrospinal fluid. This newly developed approach shows great promise for drug distribution assays including other antibiotics and can help elucidate the ADME of bitespiramycin.
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SCIENCE OF THE TOTAL ENVIRONMENT
·
2021
·
IF 7.963
Hao Xu,Qian Ye,Jing Zhang,Qiansong Li,Meijing Wang,Peng Zhou,Guanyu Zhou,Qingguo Wang
In response to the inherent restriction of low Fe(II) regeneration in the Fenton process, this study demonstrated a mutual-promoting configuration, where oxygen functionalized g-C 3 N 4 (OCN) was applied in Fe(III)/H 2 O 2 system to utilize mild natural solar light (SL) for persistent Fe(II) generation. The constructed OCN/Fe(III)/H 2 O 2 /SL system exhibited strong adaptability to various pollutants, and it well outperformed the g-C 3 N 4 (GCN) modified system and the traditional Fenton system in pollutants degradation efficiency. Compared with GCN, OCN could significantly promote the Fe(II) generation under solar light (SL), leading to more efficient H 2 O 2 activation. The characterization analyses revealed the larger surface area and enhanced charge separation of OCN, which were considered to take main responsibility for its enhanced photoactivity. The complexation of Fe(III) with the carboxyl groups of OCN also benefited the Fe(II) generation. ·OH was detected as the dominant radical responsible for metronidazole (MNZ) degradation, and its production in the OCN modified system was about twice that in the GCN modified system and the Fenton system. Moreover, the precipitation of FeO x on the OCN surface benefited the charge separation of the OCN, so that the improved OCN enabled a slight enhancement of MNZ degradation in the reuse experiments. The intermediates of MNZ degradation were analyzed based on the results of LC-MS, which provided insight into MNZ degradation pathways. This work highlighted the concept of self-improving photocatalyst, the ingenious combination of photocatalysis and Fenton-like system formed a mutual-promoting situation where the OCN and the Fenton-like system could both be improved, which endowed the configuration great potential for green and economical oxidation in environmental remediation.
研究领域:
环境科学
·
光催化
·
水处理
·
高级氧化过程
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高影响因子
ANALYTICAL CHEMISTRY
·
2022
·
IF 8.008
Hui-Yang Liao,Xuan Xiao,Rui Peng,Juan Le,Hai-Bo Wang,Shao-Ting Wang
Quantification of steroids possesses a crucial clinical value in early diagnosis and prognosis evaluation of various endocrine diseases. However, it is still challenging to realize feasible analysis of estrogens, androgens, progestogens, and corticoids within one single workflow. In this study, two derivatization reactions were newly designed for improvement: (1) acylation of phenolic hydroxyl on estrogens with isonicotinoyl chloride (INC) under the catalysis of 4-dimethylaminopyridine and (2) post-modification of oxime hydroxyl on hydroxylamine-pretreated ketosteroids with INC. Both reactions could conduct instantaneously at room temperature under aqueous conditions. Moreover, the resulting phenolic-INC and oxime-INC esters exhibited favorable MS responses. Through integrating these derivatization strategies with cold-induced phase separation technology, a feasible LC–MS/MS method was developed for simultaneous quantification of 15 multiclass steroids with proper sample consumption (50 μL serum), satisfying sensitivity (lower limit of quantitation at 0.01–5.00 ng/mL) and high throughput (40 min for sample-preparation). The practical applicability was tested by detecting 30 real samples from pregnant and non-pregnant women. The obtained results showed a good agreement with a previous validated methodology.
研究领域:
临床医学
·
分析化学
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2021
·
IF 3.205
Dan-Tong Zhao,Yi-Jun Gao,Wen-Jin Zhang,Tian-Chen Bi,Xiao Wang,Chun-Xia Ma,Rong Rong
Mycotoxins are poisonous secondary fungal toxic metabolites and harmful to human health. Traditional Chinese medicinal materials (TCMs), including more than two hundred functional foods, are vulnerably bred fungi, causing spoilage and multi-mycotoxins contamination. This study established a simultaneous analytical method by using multi-mycotoxins immunoaffinity column (multi-IAC) and HPLC-MS/MS to evaluate mycotoxins' contamination levels and natural incidence in TCMs. Aflatoxins (AFs, including AFB1, AFB2, AFG1 and AFG2), ochratoxin A (OTA), fumonisins (FB1 and FB2), zearalenone (ZEN), deoxynivalenol (DON) and T-2 toxins in three TCMs or functional foods of Polygalae Radix (PR), Coicis Semen (CS) and Eupolyphaga Steleophaga (ES) were detected. The systematically investigated results of 30 batch AFB1 positive samples revealed co-occurrence and correlation of multi-mycotoxins are significant differences in various matrices. All the samples in this study contain more than 5 mycotoxins. AFB1-AFs, AFB1-FBs, AFB1-DON, and AFB1-T-2 are the most observed co-occurrence, AFB1-OTA is also of concern due to its synergistic toxicity. This study's results can be used to establish guidelines for screening mycotoxin contaminants and limitations on acceptable levels in TCMs. Simultaneously, mycotoxin's correlation results in different matrices can also provide a reference for the standardization of TCM production and processing.
研究领域:
食品科学
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分析化学
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毒理学
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RSC Advances
·
2018
·Vol. 8
·期 30
·16645-16656
·
IF 2.936
Hua Wang,Jia-hui Hu,Cui-chai Liu,Min Liu,Zheng Liu,Li-xin Sun
In the process of anticancer drug development, research on the mechanism of action remains a major obstacle. In the present study, a cell metabolic profiling based discriminatory model was designed to give general direction on anticancer candidate mechanisms. Firstly, ultra-performance liquid chromatography in tandem with high-definition mass spectrometry was applied to obtain a comprehensive metabolic view of 12 human tumor cells. Secondly, multivariate data analysis was used to assess the metabolites’ variations, and 42 metabolites were identified as the main contributors to the discrimination of different groups. Then a metabolite-based prediction model was constructed for the first time and verified by cross validation (R2 = 0.909 and Q2 = 0.869) and a permutation test (R2 = 0.0871 and Q2 = −0.4360). To validate if the model can be applied for mechanism prediction, 4 independent sample sets were used to train the model and the data dots of different drugs were located in different regions. Finally, the model was applied to predict the anticancer mechanism of two natural compounds and the results were consistent with several other studies. Overall, this is the first experimental evidence which reveals that a metabolic profiling based prediction model has good performance in anticancer mechanism research, and thus it may be a new method for rapid mechanism screening.
研究领域:
药理学
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肿瘤学
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代谢组学
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2026
·
IF 3.8
Wang Dong,Li Mengrong,Zhang Xiangyu,Chai Shiwei,Chen Di
A novel ultrasound-assisted magnetic sorbent–wrapped stick dip extraction (UA-MSWS-DE) method was developed for the batch-scale determination of seven tyrosine kinase inhibitors (TKIs) in human plasma. The extraction device was fabricated by immobilizing octadecylphosphonic acid–functionalized magnetic nanoparticles onto flame-sealed glass capillaries embedded with magnets. Ultrasonic-assisted dip extraction was used to extract TKIs from diluted plasma, followed by quantification via liquid chromatography–tandem mass spectrometry (LC-MS/MS). Key extraction parameters were systematically optimized, yielding the following optimal conditions: sample pH 5.0 and volume 1.0 mL, sorbent particle size 20 nm and dosage 10 mg, extraction time 20 min, and desorption with 150 µL of ethanol for 8 min. The method demonstrated excellent linearity ( R 2 ≥ 0.99), low limits of quantification (0.1–5.0 ng/mL), and good intra-/inter-day precision (RSDs < 14.95%). The accuracy in blinded plasma samples, tested at 0.25–25% of the studied concentration range, ranged from 87.13 to 112.33%. Compared to conventional magnetic dispersive solid-phase extraction, the UA-MSWS-DE strategy simplifies handling and is designed to facilitate potential parallel processing using only an ultrasonic bath. Five greenness metrics confirmed the method’s high sustainability. Furthermore, the modular design enables adaptation to other analytes by modifying the sorbent coating, making UA-MSWS-DE a sensitive, green, and automation-ready method for therapeutic drug monitoring. Graphical
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2018
·Vol. 32
·期 12
·e4373
·
IF 1.688
Qi Wen,Hai-Long Li,Feng Chen,Jing-Wen Gong,Wei-Wei Guan,Nai-Guang Fu,Yin-Feng Tan
The aim of the present study was to develop a rapid, specific and sensitive LC–MS/MS method for the determination of DPHB [7-(4″-hydroxy-3″-methoxyphenyl)-1-phenyl-4-hepten-3-one] in rat plasma using yakuchinone A as an internal standard (IS). n -Hexane was used for the extraction of DPHB from rat plasma. Chromatographic separation of DPHB was achieved using a Kinetex XB-C 18 column (2.10 × 50 mm, 2.6 μm) at 40°C. The mobile phase consisted of water (containing 0.1‰ formic acid, A) and acetonitrile (containing 0.1‰ formic acid, B) under a gradient elution at a flow rate of 0.3 mL min −1 . Positive electrospray ionization and multiple reaction monitoring mode were used for detection. The selected precursor ion to product ion pairs, m / z 311.3 → 137.0 for DPHB and m / z 313.1 → 137.0 for yakuchinone A, were monitored. Good linearity was observed over the concentration range from 2 to 2000 ng mL −1 ( r = 0.9969). The recovery efficiency of DPHB from rat plasma was 54.8–69.7%, while the matrix effect ranged from 99.7 to 113%. Intra- and inter-day precision and accuracy values were within ±15% at three different quality control concentration levels. This validated method was successfully applied to pharmacokinetic studies in rats after a single p.o. or i.v. dose of DPHB solution. The route of administration significantly influenced systemic exposure to DPHB, and low bioavailability of DPHB was observed. The method developed here will be further improved and used in future pharmacokinetic studies.
研究领域:
分析化学
·
药学
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药代动力学
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生物分析
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高影响因子
FOOD CHEMISTRY
·
2026
·
IF 10.4
Xia Xu,Chen Liang,Zengbo Fang,Ting Zhao,Mingjie Liu,Yan Cui
A novel chiral derivatization reagent {DMT-OTZD-3( S )-Apy} was synthesized. • A sensitive LC-MS/MS method was developed for the simultaneous determination of six NSAID enantiomers. • Determination of NSAID enantiomers was carried out firstly in multi-specie meat products. In stock farming, illegal use of non-steroidal anti-inflammatory drugs has caused food safety problems. A novel chiral derivatization reagent targeted carboxyl groups, ( S )-[(( R )-1-(4,6-dimethoxy-1,3,5-triazine-2-yl)-2-oxothiazolidine-4‑carbonyl] pyroli-dine-3-amine {DMT-OTZD-3( S )-Apy}, was synthesized. After derivatization with it, the first multi-residue and simultaneous determination targeted six NSAID enantiomers in beef and mutton products was conducted. The method was validated to be selective, and got an excellent linear relationship for all enantiomers within their respective concentration ranges ( r 2 ≥ 0.9990). The average recoveries were from 91.7% to 104.3%, and the RSDs corresponding to intra-day and inter-day precision did not exceed 6.2%. The limit of detections spanned the interval of 0.30–1.42 ng/g, which were far lower than maximum residue limits established by China and the European Union. The method would provide methodology support for the risk assessment of NSAIDs in meat products from enantiomeric levels. Download: Download high-res image (122KB) Download: Download full-size image
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2026
·
IF 3.4
Yue Shi,Fangqi Cao,Xin Bai,Xia Ran,Xiaoliang Yuan,Daiwen Zhang,Zhiru Xu,Chaojun Li
Validated LC-MS/MS for 4-MEC, M1 and M2 in whole blood • Applied to IV and intragastric pharmacokinetic study • First in vivo PK characterization of 4-MEC and major metabolites • M2 shows prolonged exposure and extended detection window 4-Methyl- N -ethylcathinone (4-MEC) is a novel psychoactive substance and its in vivo exposure characterization remains unknown. In this study, a sensitive and robust liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and fully validated for the simultaneous quantification of 4-MEC and its two major metabolites in rat whole blood. Then it was applied to pharmacokinetic studies of 4-MEC in rats by intravenous and intragastric administration, characterizing the concentration-time profiles of the parent compound and its metabolites. The results revealed distinct exposure patterns between 4-MEC and its metabolites. Notably, M2 ( N -deethylated metabolite) exhibited a prolonged detection window compared with 4-MEC, supporting metabolite-based monitoring strategies and thereby extending its application in forensic toxicology and drug abuse identification.
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2025
·
IF 3.1
Lili Liu,Yaping Huang,Qingqing Wang,Ziyuan Wang,Ke Pan,Jian Zhang,Ying Peng,Guangji Wang,Zhiqi Yin,Jianguo Sun
As a plant with a rich history of medicinal and dietary use, Gynostemma pentaphyllum (Thunb.) Makino is predominantly characterized by the gypenosides. Contemporary research has demonstrated that these saponins possess significant hypolipidemic and hypoglycemic effects. This study focused on developing an LC-MS/MS approach to elucidate the pharmacokinetic profiles of 13 gypenosides in rat models. The separation was accomplished using a ZORBAX Eclipse Plus C18 column (2.1 mm × 100 mm, 1.8 µm). Detection was facilitated by employing positive electrospray ionization (ESI) in multiple reaction monitoring (MRM) mode. The analytical method was fully validated, including selectivity, linear response, measurement precision, analytical accuracy, extraction efficiency, matrix interference, and sample stability. The lower limit of quantification (LLOQ) for all compounds was 10 ng/mL, with each exhibiting a favorable linear relationship (r ≥ 0.9960). The precision, as measured by the relative standard deviation (RSD) for intra-day and inter-day variability, did not exceed 8.41 %. The accuracy, expressed as the relative error (RE), varied from −4.42–8.42 %. The recovery rate of the extraction process was between 92.02 % and 114.77 %, and no notable matrix effects were detected. The stability of the compounds was confirmed under four distinct storage conditions. Pharmacokinetic results indicated that all analytes displayed rapid absorption, prolonged retention, and slow elimination in rats, and exhibited nonlinear pharmacokinetics at low, medium, and high dosage levels. This study has established a quantification method for 13 gypenosides and successfully applied it to their pharmacokinetic studies in rats, providing a foundation for their further development and utilization.
研究领域:
中药学
·
分析化学
·
药理学
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高影响因子
危险品化学品经营许可证（带存储）