Scientific Reports
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2024
·Vol. 14
·期 1
·1-18
·
IF 3.8
Zhang Jing,Xin Hongmei,Wang Wuji,Li Yanyi,Wu Riga,Wei Lisi,Su Si,Wang Xiaohong,Wang Xiujuan,Wang Xiaojuan,Li Li,Hu Rilebagen
Lactoferrin is a natural multifunctional glycoprotein with potential antidepressant-like effects. However, the mechanism of its antidepressant effect has not been explored from the perspective of gut flora metabolism. Therefore, we employed both 16S rDNA gene sequencing and LC–MS metabolomics analysis to investigate the regulatory effects and mechanisms of lactoferrin in a rat model of depression. After one week of acclimatization, twenty-four 7-week-old male Sprague–Dawley rats were randomly and equally assigned into three groups: the control group, the model group, and the lactoferrin intervention group. The control group rats were housed under standard conditions, while the rats in the model and lactoferrin intervention groups were individually housed and exposed to chronic unpredictable mild stress for 44 days simultaneously. The lactoferrin intervention group was provided with water containing 2% lactoferrin (2 g/100 ml). Behavioural tests were conducted at week 7. Upon completion of the behavioral tests, the rats were anesthetized with isoflurane, humanely euthanized using a rat guillotine, and tissue samples were collected for further experiments. The results indicated that lactoferrin intervention led to an increase in sucrose solution consumption, horizontal movement distance, number of cross platforms, and residence time in the target quadrant. Additionally, it resulted in an increase in jejunal tight junction protein ZO-1 expression and a suppression of serum expression of inflammatory factors, Lipopolysaccharide and Diamine oxidase. In summary, lactoferrin can regulate the metabolic disorder of intestinal flora, reduce intestinal permeability, and further regulate the metabolic balance of hippocampal tissues through the microbiota-gut-brain axis. This process ultimately alleviates the depression-like behavior in rats.
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JOURNAL OF CHROMATOGRAPHY A
·
2025
·
IF 4
Fuyang Gu,Xiaoyan Wang,Jinmei Du,Yang Jiang,Dagang Miao,Yanmei Qu,Dongyan Shao,Guowei Xiao,Changhai Xu
Cationic bleaching activators can effectively achieve low-temperature bleaching in hydrogen peroxide system, but at the same time, self-hydrolysis reaction will occur to affect the low-temperature bleaching effect, and the complex hydrolysis pathways of cationic bleaching activators are still elusive. In this paper, the hydrolysis reaction pathways, mechanisms, rates and kinetics of cationic bleaching activators N-[4-(triethylaminomethyl)benzoyl]lactam chlorides (TBLCs) with different lactam leaving groups were investigated in depth by liquid chromatography-mass spectrometry (LC-MS) and high-performance liquid chromatography (HPLC). Specifically, we characterized the hydrolysis products by LC-MS and further quantified the hydrolysis products using HPLC, demonstrating that the hydrolysis can take place via two pathways, generating chain-breaking products and ring-opening products, and that both react at different rates depending on the different lactam leaving groups. Notably, the quantitative results showed that the chain-breaking products were always larger than the ring-opening products, and the chain-breaking products were ineffective for bleaching, which was the main reason for the decrease in the bleaching performance of TBLCs. The mechanism of hydrolysis is discussed and the reaction rate was determined to follow first-order kinetics using HPLC. We have successfully delineated the complete transformation pathway of the hydrolysis reaction using this method, providing valuable information for the future preparation of novel bleaching activators and the reduction of this reaction.
研究领域:
化学工程
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分析化学
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INTERNATIONAL JOURNAL OF MOLECULAR SCIENCES
·
2026
·Vol. 27
·期 13
·5821
·
IF 5.6
Huaxin Cai,Wenzhe Li,Dongxu Wang,Canxia Wu,Jingyang Ni,Yinghua Tong
The red imported fire ant (Solenopsis invictaBuren) is a destructive invasive pest, and conventional chemical control faces challenges related to environmental contamination and resistance development, highlighting the need for novel control agents and greener management strategies. In this study, pyrethrins-mediated silver nanoparticles (Pyr-AgNPs) were synthesized via a green route, characterized, and evaluated for their insecticidal activity, environmental stability, and metabolic effects onS. invictaworkers. Bait bioassays showed that Pyr-AgNPs exhibited high toxicity toS. invicta, causing 100% cumulative corrected mortality at 500 mg·kg−1after 9 days of feeding, with a 5-d LC50of 116.83 mg·kg−1. Exposure assays further demonstrated that Pyr-AgNPs had good environmental stability and residual efficacy, as bait containing 1000 mg·kg−1Pyr-AgNPs still caused 100% cumulative corrected mortality after 9 days following 96 h of outdoor exposure, significantly outperforming the pyrethrins treatment. LC-MS-based untargeted metabolomic analysis revealed that treatment with Pyr-AgNPs markedly altered the metabolic profile ofS. invictaworkers, with 607 differential metabolites identified, mainly belonging to organic acids and derivatives, lipid and lipid-like molecules, amino acids and peptides, cofactors, and redox-related metabolites. Pathway enrichment analysis indicated that these metabolic disturbances were primarily associated with energy metabolism, redox homeostasis, and membrane lipid metabolism. Overall, these findings provide preliminary mechanistic clues into the toxicity of Pyr-AgNPs and support their potential application in the sustainable management ofS. invicta.
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CLINICA CHIMICA ACTA
·
2026
·
IF 4.1
Zhenni Liu,Xiaohua Xiao,Bingchu Li,Nijiao Qin,Ziyang Li,Xing Lyu,Zhongyuan Xiang,Min Hu,Qichen Long
A rapid and practical LC-MS/MS method for ascitic-fluid CK18 quantification. • Sequential salting-out/pI-guided acidic precipitation strategy for CK18 enrichment. • Simplified pretreatment shortens overall sample preparation duration to merely 6 h. • Ascitic-fluid CK18 correlates with hepatic markers for auxiliary cirrhosis evaluation. Cytokeratin 18 (CK18), a predominant hepatocyte intermediate filament protein released during hepatocyte death, has been investigated as a hepatic injury biomarker. Conventional immunoassays for CK18 suffer from non-specific cross-reactivity and insufficient standardization. Though liquid chromatography-tandem mass spectrometry (LC-MS/MS) could overcome such immunoanalytical drawbacks, accurate CK18 quantification in ascitic fluid remains analytically challenging because of the complex matrix, low target abundance, and variability introduced by protein enrichment and digestion. Herein, we developed a rapid and practical LC-MS/MS method for CK18 quantification in ascitic fluid. A two-step non-immunoaffinity enrichment strategy, integrating sequential ammonium sulfate salting-out and isoelectric point-driven acidic precipitation, was optimized to balance enrichment yield, pretreatment turnaround, and operational cost. Subsequent pretreatment workflow comprising urea denaturation, enzymatic hydrolysis, and solid phase extraction purification can be completed within 6 h, providing an economical, instrument-compatible procedure for LC-MS/MS analysis. Systematic analytical performance evaluation showed satisfactory linearity spanning 0.10–10.36 nmol/L, a limit of quantification of 0.10 nmol/L, a limit of detection of 0.02 nmol/L, total imprecision <10%, and recoveries ranging from 93.07% to 108.92%. The internal standard effectively compensated for LC-MS/MS instrumental variability and ionization-related matrix effects. Method comparison showed acceptable agreement with a published multiplexed cytokeratin MS method. Clinical analysis demonstrated significantly elevated ascitic-fluid CK18 concentration in cirrhotic patients versus non-cirrhotic controls ( P = 0.001). This novel enrichment strategy preserves the simplicity and cost-efficiency of conventional precipitation methods while avoiding costly antibody capture reagents. Collectively, the validated LC-MS/MS method is appropriate for preliminary exploration of the clinical value of ascitic-fluid CK18 and can facilitate translational research in cirrhotic populations.
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FOOD CHEMISTRY
·
2026
·
IF 10.4
Mohan Li,Chenhao Jiang,Dian Zhou,Kewei Chen,Muying Du,Zsolt Zalán,Sameh Awad,Jianquan Kan
A multi-technique framework dissects AFB1 matrix interference in PPC. • Demonstration of a strong solvent-dependent matrix interference in AFB1 extraction. • Non-targeted metabolomics revealed solvent-specific co-extract profiles. • Acetonitrile/water (80:20) achieved >90% recovery with minimal interference. • Distinct AFB1 interaction modes underlie stage-dependent solvent efficacy. Pressed peanut cake (PPC) is a valuable plant-based protein source, but its complex matrix might lead to underestimation of aflatoxin B1 (AFB1). This study established a multi-technique diagnostic framework integrating UV–Vis, FTIR, LC–MS/MS, and SEM to systematically dissect matrix interference in different extraction solvents, ultimately correlating with AFB1 detection. It was found that, due to lipid interference, the use of nonpolar solvents during extraction not only significantly amplified detection errors but also severely compromised extraction efficiency, resulting in an analytical error exceeding 85%. Systematic profiling revealed that conventional methanol/water extraction introduced dual errors, attributable to either inefficient toxin extraction or excessive pigment co-extraction, leading to an AFB1 underestimation up to 50%. Acetonitrile/water was identified as the optimal extraction solvent, minimizing interferents and achieving consistent AFB1 recoveries >90%. This work not only provides a practically applicable detection protocol but also offers a clear mechanistic explanation for the observed errors. Download: Download high-res image (219KB) Download: Download full-size image
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Drug Design Development and Therapy
·
2026
·
IF 6.1
Huanchen Li,Hongkun Wu,Shouhong Gao,Lili Cui,Jingjie Xu,Jianguo Sun,Zhijun Liu,Zhipeng Wang,Xia Tao
Objective Atorvastatin is frequently used in combination with almonertinib in lung cancer patients who present with comorbid dyslipidemia. Both drugs are metabolized by CYP3A4, potentially leading to drug-drug interactions (DDIs) that increase the risk of adverse reactions. This study aimed to develop a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for quantifying almonertinib and atorvastatin and evaluate the DDIs between these two drugs in rats.Methods An LC-MS/MS method was developed to determine almonertinib and atorvastatin in rat plasma and was fully validated in accordance with the ICH M10 bioanalytical method validation guideline and Chinese Pharmacopoeia 2020 Edition. Rats were divided into 5 groups (n=7 per group), and received the following treatments: almonertinib alone, atorvastatin alone, almonertinib combined with atorvastatin, vehicle control, or almonertinib after a long-term regimen of atorvastatin. The plasma samples were collected from each rat and analyzed using this method. The pharmacokinetic parameters were calculated and the DDIs were evaluated.Results An LC-MS/MS method was established and validated according to the requirements. Animal studies revealed that co-administration of almonertinib with atorvastatin significantly increased Cmax, AUC0-t, and AUC0-∞ (all p < 0.05), prolonged t1/2 (p < 0.05) and decreased CLz/F, Vz/F (both p < 0.05) of both drugs. Following a 7-day administration of atorvastatin, the DDIs between the two drugs generally weakened, but still differed significantly from those observed with single-drug administration.Conclusion The study successfully established an LC-MS/MS method for simultaneous determination of almonertinib and atorvastatin and assessed the DDIs of these two drugs in rat. Animal experiment demonstrated significant DDIs between two drugs no matter single dose or multiple doses were administered, which obviously increased the drug exposure and inhibited elimination. Close attention should be paid to the combination regimens of these two drugs in clinical practice.
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METHODS
·
2024
·
IF 4.2
Sisi Gong,Qingshui Wang,Jiewei Huang,Rongfu Huang,Shanshan Chen,Xiaojuan Cheng,Lei Liu,Xiaofang Dai,Yameng Zhong,Chunmei Fan,Zhijun Liao
Background Breast cancer (BC), the most common form of malignant cancer affecting women worldwide, was characterized by heterogeneous metabolic disorder and lack of effective biomarkers for diagnosis. The purpose of this study is to search for reliable metabolite biomarkers of BC as well as triple-negative breast cancer (TNBC) using serum metabolomics approach. Methods In this study, an untargeted metabolomics technique based on ultra-high performance liquid chromatography combined with mass spectrometry (UHPLC-MS) was utilized to investigate the differences in serum metabolic profile between the BC group (n = 53) and non-BC group (n = 57), as well as between TNBC patients (n = 23) and non-TNBC subjects (n = 30). The multivariate data analysis, determination of the fold change and the Mann-Whitney U test were used to screen out the differential metabolites. Additionally, machine learning methods including receiver operating curve analysis and logistic regression analysis were conducted to establish diagnostic biomarker panels. Results There were 36 metabolites found to be significantly different between BC and non-BC groups, and 12 metabolites discovered to be significantly different between TNBC and non-TNBC patients. Results also showed that four metabolites, including N-acetyl-D-tryptophan, 2-arachidonoylglycerol, pipecolic acid and oxoglutaric acid, were considered as vital biomarkers for the diagnosis of BC and non-BC with an area under the curve (AUC) of 0.995. Another two-metabolite panel of N-acetyl-D-tryptophan and 2-arachidonoylglycerol was discovered to discriminate TNBC from non-TNBC and produced an AUC of 0.965. Conclusion This study demonstrated that serum metabolomics can be used to identify BC specifically and identified promising serum metabolic markers for TNBC diagnosis.
研究领域:
肿瘤学
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代谢组学
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生物信息学
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临床诊断
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高影响因子
JOURNAL OF LIPID RESEARCH
·
2020
·Vol. 61
·期 4
·580-586
·
IF 4.483
Teng-Fei Yuan (袁;腾;飞,Juan Le (乐;娟,Shao-Ting Wang (王;少;亭,Yan Li (李;艳
Analyzing global steroid metabolism in humans can shed light on the etiologies of steroid-related diseases. However, existing methods require large amounts of serum and lack the evaluation of accuracy. Here, we developed an LC/MS/MS method for the simultaneous quantification of 12 steroid hormones: testosterone, pregnenolone, progesterone, androstenedione, corticosterone, 11-deoxycortisol, cortisol, 17-hydroxypregnenolone, 17-hydroxyprogesterone, dehydroepiandrosterone, estriol, and estradiol. Steroids and spiked internal standards in 100 μl serum were extracted by protein precipitation and liquid-liquid extraction. The organic phase was dried by evaporation, and isonicotinoyl chloride was added for steroid derivatization, followed by evaporation under nitrogen and redissolution in 50% methanol. Chromatographic separation was performed on a reverse-phase PFP column, and analytes were detected on a triple quadrupole mass spectrometer with ESI. The lower limits of quantification ranged from 0.005 ng/ml for estradiol to 1 ng/ml for cortisol. Apparent recoveries of steroids at high, medium, and low concentrations in quality control samples were between 86.4% and 115.0%. There were limited biases (−10.7% to 10.5%) between the measured values and the authentic values, indicating that the method has excellent reliability. An analysis of the steroid metabolome in pregnant women highlighted the applicability of the method in clinical serum samples. We conclude that the LC/MS/MS method reported here enables steroid metabolome analysis with high accuracy and reduced serum consumption, indicating that it may be a useful tool in both clinical and scientific laboratory research.
研究领域:
临床医学
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分析化学
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Toxics
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2025
·Vol. 13
·期 5
·352
·
IF 4.1
Yubing Yan,Bowen Liang,Jiawen Yang,Qing Deng,Xiaoying Liang,Hui Chen,Bibai Du,Lixi Zeng
Fluorescent brighteners (FBs) are a class of chemicals extensively used in industrial and consumer products. Their environmental occurrences and potential health risks have raised significant concerns. However, the lack of analytical methods for FBs in human samples has hindered the accurate assessment of internal exposure levels. Addressing this gap, this study developed and validated a novel method for the simultaneous determination of 13 FBs at trace levels in human plasma using solid-phase extraction combined with HPLC-MS/MS. The method employed EMR-Lipid SPE columns, which can selectively adsorb phospholipids for plasma sample pre-treatment. Detection was achieved through positive ion electrospray ionization (ESI) in multiple reaction monitoring (MRM) modes. The results showed that all 13 FBs exhibited good linearity within their respective ranges, with correlation coefficients (R2) greater than 0.992. The method quantitation limits (MQLs) of the FBs ranged from 0.012 to 0.348 ng/mL, and the spiked recovery rates ranged from 61% to 98%. The method was successfully applied to analyze 10 adult plasma samples, detecting 10 FBs with total concentrations ranging from 0.221 to 0.684 ng/mL. This study provides a reliable analytical method for determining FBs in human plasma, providing a basis for further research on human internal exposure to FBs and associated health risk assessments.
研究领域:
分析化学
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环境健康学
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毒理学
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2019
·
IF 2.813
Jian Ren,Chang-Liang Hu,Zheng-Ping Zhang,Rong Chen,Shi-Bao Yang,Zhen-Yu Miao,Lu-Ning Sun,Yong-Qing Wang
(+)-Borneol, a bicyclic monoterpene , has been shown to possess valuable biological properties and potential as a pharmaceutical agent due to anti-inflammatory, anti-oxidant and GABA receptor-enhancing functions; it also enhances the permeability of the blood brain barrier to improve the efficacy of CNS drugs. In this study, we have developed a simple, selective, and rapid liquid chromatography-tandem mass spectrometry method for the assay of (+)-borneol in rat plasma. Verapamil was used as an internal standard. Plasma samples were deproteinized using methanol. The analyte was detected by a mass spectrometer with positive atmospheric pressure chemical ionization by multiple reaction monitoring mode for transitions at m / z [M + H] + 137.2 → 81.0 for (+)-borneol and 455.2 → 165.1 for verapamil. The method has been fully validated to ensure good selectivity, a satisfactory lower limit of quantification at 10.0 ng/mL, acceptable intra- and inter-day accuracy, and high precision. The method was used for the pharmacokinetic evaluation of (+)-borneol in Sprague-Dawley rats after intravenous, oral, and sublingual administration. The results indicate that oral bioavailability of (+)-borneol was extremely low but sublingual administration yielded rapid absorption and favorable bioavailability of (+)-borneol.
研究领域:
药理学
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分析化学
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药物代谢
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高影响因子
INTERNATIONAL JOURNAL OF MOLECULAR SCIENCES
·
2024
·Vol. 25
·期 7
·3654
·
IF 4.9
Wencheng Zhao,Huizi Cui,Kaifeng Liu,Xiaotang Yang,Shu Xing,Wannan Li
Type 2 diabetes mellitus (T2DM) is marked by persistent hyperglycemia, insulin resistance, and pancreatic β-cell dysfunction, imposing substantial health burdens and elevating the risk of systemic complications and cardiovascular diseases. While the pathogenesis of diabetes remains elusive, a cyclical relationship between insulin resistance and inflammation is acknowledged, wherein inflammation exacerbates insulin resistance, perpetuating a deleterious cycle. Consequently, anti-inflammatory interventions offer a therapeutic avenue for T2DM management. In this study, a herb called Baikal skullcap, renowned for its repertoire of bioactive compounds with anti-inflammatory potential, is posited as a promising source for novel T2DM therapeutic strategies. Our study probed the anti-diabetic properties of compounds from Baikal skullcap via network pharmacology, molecular docking, and cellular assays, concentrating on their dual modulatory effects on diabetes through Protein Tyrosine Phosphatase 1B (PTP1B) enzyme inhibition and anti-inflammatory actions. We identified the major compounds in Baikal skullcap using liquid chromatography–mass spectrometry (LC–MS), highlighting six flavonoids, including the well-studied baicalein, as potent inhibitors of PTP1B. Furthermore, cellular experiments revealed that baicalin and baicalein exhibited enhanced anti-inflammatory responses compared to the active constituents of licorice, a known anti-inflammatory agent in TCM. Our findings confirmed that baicalin and baicalein mitigate diabetes via two distinct pathways: PTP1B inhibition and anti-inflammatory effects. Additionally, we have identified six flavonoid molecules with substantial potential for drug development, thereby augmenting the T2DM pharmacotherapeutic arsenal and promoting the integration of herb-derived treatments into modern pharmacology.
研究领域:
药理学
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糖尿病研究
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草药医学
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生物化学
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分子生物学
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ANALYTICA CHIMICA ACTA
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2025
·
IF 6
Shiwen Zhou,He Tang,Lu Gao,Wangyu Li,Jiancong Liao,Xihe Yang,Yuanjiang Pan,Hongru Feng
Background Oligonucleotide-based drugs have gained significant attention as a promising class of therapeutics due to their precise ability to regulate gene expression. However, the presence of impurities in these drugs can compromise their safety, efficacy, and stability. Therefore, the identification and detailed analysis of these impurities are crucial. Traditional methods may struggle to detect subtle impurities, such as oxidation and hydrolysis products, which necessitate the development of more advanced and reliable analytical techniques for oligonucleotide therapeutics. Results In this study, we introduce a novel analytical method that combines heart-cutting two-dimensional liquid chromatography (2D-LC) with tandem mass spectrometry (MS/MS) to effectively separate, analyze, and identify impurities in oligonucleotide-based drugs. The first dimension utilizes anion exchange chromatography (AEX) to separate oligonucleotides based on their negative charge, while the second dimension employs reverse ion-pair chromatography (RIPC) for further purification and compatibility with mass spectrometry. This 2D-LC-MS/MS approach provides a sensitive and accurate means of identifying and quantifying impurities, including oxidation and hydrolysis products. The method was applied to two RNA interference (RNAi) drugs, Givosiran and Patisiran, where 3 and 20 impurities were identified, respectively. Additionally, sequencing analysis using data-dependent acquisition (DDA-MS/MS) enabled the determination of the molecular weight and structural characteristics of these impurities, offering a comprehensive and detailed view of the impurity profiles. Significance This novel heart-cutting 2D-LC-MS/MS method offers a significant advancement in the analysis of impurities in oligonucleotide-based therapeutics. It provides high sensitivity, enabling the identification of subtle impurities that are often challenging to detect. By applying this technique to RNAi drugs, we demonstrate its potential to enhance the safety, efficacy, and stability of oligonucleotide-based therapies, making it a valuable tool for the pharmaceutical industry.
研究领域:
药物分析
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分析化学
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生物治疗学
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质谱分析
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色谱分析
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药物研发
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生物药剂学
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高影响因子
危险品化学品经营许可证（带存储）