FITOTERAPIA
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2025
·
IF 2.6
Xuan Zhang,Jie Weng,Yi Luo,Hongcun Liu,Jing Yan,Zhiqiang Gong,Chaonan Kong,Xue Li,Lifang Yang,Mingguo Jiang
To elucidate the efficacy and potential molecular mechanisms underlying the therapeutic effects of Spatholobi Caulis flavonoids (SCF) in the treatment of primary dysmenorrhea (PD). The present study established oxytocin-induced uterine contractions in vitro and a model of PD in rats evoked by estradiol benzoate and oxytocin. The uterine contraction experiments demonstrated that SCF significantly inhibited uterine smooth muscle tone by 62.07 %. SCF effectively attenuated the torsional response in PD rats, normalised the PGF2α/PGE2 ratio, and reduced NO and Ca 2+ levels. The constituents of SCF were evaluated by using a Liquid Chromatograph Mass Spectrometer(LC-MS) method, and 11 flavonoid components were preliminarily deduced. Network pharmacology and molecular docking (MD) techniques were used to predict therapeutic targets, with the former suggesting key targets such as RhoA, VEGFA, and PIK3CA, while the latter indicated that 10 compounds had a strong binding affinity for RhoA. The expression of CALM, RhoA, ROCK1, PIK3CA, and AKT was down-regulated at both the protein and mRNA levels. Additionally, the expression levels of genes associated with VEGFA, IP3R, MLCK and NOS3 were found to be regulated. The collective evidence from this study suggests that SCF may attenuate uterine spasm by inhibiting the RhoA/ROCK signaling pathway, decreasing the levels of PGF2α, NO and Ca 2+ , and increasing the content of PGE2. This study provides a theoretical basis for the application of SCF in the treatment of PD.
研究领域:
药理学
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分子生物学
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2025
·Vol. 39
·期 6
·e70108
·
IF 1.7
Ancheng Gu,Chuwen Zhang,Dan Li,Bohong Cen,Wanwen Cao,Zhongyuan Xu
Dapagliflozin is a widely used sodium-glucose cotransporter 2 inhibitor that has been approved for the treatment of Type 2 diabetes. In this study, we present a simple and sensitive high-performance liquid chromatography tandem mass spectrometry (HPLC–MS/MS) method for the simultaneous quantification of dapagliflozin and its metabolite, dapagliflozin 3-O-glucuronide (D3OG). The experiments were conducted using an Agilent G6495B triple quadrupole mass spectrometer coupled with an Agilent 1290 Infinity II HPLC system, featuring a Poroshell 120 EC-C18 column. Gradient elution was performed with ammonium formate (10 mM) and methanol as the mobile phase. The G6495B was operated in negative ion mode with electrospray ionization and multiple reaction monitoring. The quantitative method was validated according to FDA and EMA guidelines, assessing parameters such as selectivity, linearity, accuracy, precision, dilution integrity, stability, and recovery. Methanol was used as a protein precipitant during sample preparation, resulting in consistent extraction recoveries ranging from 91% to 96% for all analytes. The linear range for the analytes was established at 2–800 μg/L with a sample volume of 100 μL. This validated method is sufficient for the simultaneous quantification of dapagliflozin and D3OG in plasma and has been successfully applied in pharmacokinetic studies, bioequivalence assessments, and clinical therapeutic monitoring. Trial Registration: Chinese Clinical Trial identifier: ChiCTR2100044600
研究领域:
分析化学
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药理学
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临床医学
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JOURNAL OF FOOD COMPOSITION AND ANALYSIS
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2025
·
IF 4.6
Cong Liu,Yanli Dong,Junmin Wang,Qianqian Wang,Chun Wang,Qiuhua Wu
Phenolic environmental endocrine disruptors (EEDs) pose significant risks to the reproductive and nervous systems. Herein, we synthesized a magnetic OH-anchored porous polymer (M-Pue@TB-HCP2) by linking natural puerarin with 1,3,5-tris(bromomethyl)benzene for the first time. M-Pue@TB-HCP2 showed high extraction recovery (94 %-99 %) for phenolic EEDs (bisphenol S, bisphenol A, bisphenol B and p -tert-butylphenol) thanks to its amphiphilic sites supplying hydrogen bonding and π conjugation interaction. Moreover, M-Pue@TB-HCP2 displayed excellent reusability and long service life. Using M-Pue@TB-HCP2 as magnetic solid-phase extraction adsorbent, coupled with high-performance liquid chromatography-mass spectrometry, a novel method was established for detecting trace EEDs from shrimps, achieving low detection limit (0.80–5.50 ng g −1 for green shrimp, 1.00–4.00 ng g −1 for white shrimp), good spiked recovery of 80.3 %-117 %, relative standard deviation less than 5.7 %. The method has the merits of high sensitivity, good accuracy and excellent reproducibility, making it suitable for the trace analysis of EEDs in shrimps. This work not only provides a new option for rapid and accurate detection of trace EEDs in shrimps but also explores a new strategy for the preparation of efficacious adsorbents by utilizing sustainable raw materials.
研究领域:
环境科学
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高分子化学
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分析化学
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食品安全
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内分泌学
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纳米技术
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吸附技术
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ANALYTICA CHIMICA ACTA
·
2025
·
IF 6
Yuling Li,Weiran Zhao,Xiang Xiang,YunLei Hu,Xiaoqiang Zhang,Wenjian Sun,Xiaoxuan Liu
Background Perturbed lipid metabolism in cellular environment plays an essential role in the progression of peripheral neuropathy, such as Charcot-Marie-Tooth disease type 1A (CMT1A). Current deep-profiling of lipidome still has certain limitations for high-throughput analysis of clinical samples, such as low sensitivity, extensive requirement of instrument modification, technician-dependent pretreatment and lack of method-adapted data-processing software. Results Herein, a new generation aza-Prilezhaev aziridination (APA) reagent has been designed for coupling with high-resolution liquid chromatography mass spectrometry (LC-MS) to conduct comprehensive untargeted deep lipidomics of CMT1A disease. It facilitates large-scale lipid structural annotations over a wide polarity range in a single run with high-sensitivity. With the developed method, an extensive library containing information on retention time, m / z , and MS/MS down to C=C location levels for 393 unsaturated lipids of CMT1A was created. Significant disease-related differences in C=C isomer profiles were observed from the comparison of plasma between CMT1A patients (N=9) and controls (N=8). Specifically, 40 different lipids were identified, predominantly comprising n-6, n-7, and n-9 C=C positional isomers. Significance This innovative methodology would offer substantial potential to enhance diagnosis and therapeutic strategies for CMT1A and other diseases based on lipid isomerization information.
研究领域:
神经病学
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脂质组学
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代谢组学
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分子诊断学
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FOOD RESEARCH INTERNATIONAL
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2023
·
IF 8.1
Yingyi Huang,Huahong Liu,Xiaohua Zhang,Yuxin Wu,Zhusheng Liu,Yuelan Pang,Renjun Liu,Chun Yang,Jinfang Nie
Long-term storage of Liupao tea (LPT) is usually believed to enhance its quality and commercial value. The non-volatile metabolites variations and the fungal succession play a key role for organoleptic qualities during the storage procedure. To gain in-depth understanding the impact of storage time on the quality of LPT, two different brands of LPT with different storage time, including Maosheng LPTs (MS) with 0, 5, 10 and 15 years and Tianyu LPTs (TY) with 0, 3, 5, 8 and 10 years, were resorted to investigate the changes of non-volatile metabolites and fungi as well as their correlation by multi-omics. A total of 154 and 119 differential metabolites were identified in these two different brands of MS and TY, respectively, with the aid of high-performance liquid chromatography with quadrupole-time-of-flight mass spectrometry. In both categories of LPTs, the transformation of differential metabolites in the various stages referred to the formation of alkaloids, increase of organic acids, biosynthesis of terpenoids as well as glycosylation and methylation of flavonoids. Thereinto, glycosylation and methylation of flavonoids were the critical stages for distinguishing MS and TY, which were discovered in MS and TY stored for about 10 and 8 years, respectively. Moreover, the results of high-throughput sequencing showed that the key fungal genera in the storage of LPTs consisted of Eurotium , Aspergillus , Blastobotrys , Talaromyces , Thermomyces and Trichomonascus . It was confirmed on the basis of multivariate analysis that the specific fungal genera promoted the transformation of metabolites, affecting the tea quality to some extent. Therefore, this study provided a theoretical basis for the process optimization of LPT storage.
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2020
·
IF 3.209
Yanfei Chen,Zhaoliang Hu,Wenzhu Qi,Shuxiao Gao,Jing Jiang,Shixiao Wang,Lei Xu,Xin Xu,Min Song,Taijun Hang
Chinese herbal drugs are often combined with chemotherapy drugs for the treatment of cancers. However, the combination administrations often do not have scientifically sound bases established on full preclinical and clinical investigations. A commonly used anti-colon-cancer herb-drug pair, irinotecan (CPT-11) hydrochloride injection and Kang’ai (KA) injection was taken as an example to investigate the possible pharmacokinetic interactions between Chinese herbal drugs and chemotherapy injections to determine the potential adverse drug reactions (ADRs). Rats were randomly divided into three groups and received 20 mg/kg CPT-11 injection 15 min after administration of 4 mL/kg saline for the CPT-11 single administration group and 4 mL/kg KA injection for the separated co-administration group, respectively. In the pre-mixed co-administration group, rats received a mixture of 20 mg/kg CPT-11 injection and 4 mL/kg KA injection. Blood samples were collected at 10 pre-determined time points between 0 and 24 h. The tissue samples were collected at 5 and 8 min after the injections, respectively. A reliable LC–MS/MS method was established for the simultaneous determination of CPT-11 and its metabolites, SN-38, SN-38 G and APC in the rat plasma and tissue samples, after full confirmation of two injections chemical and stability compatibilities. Compared to the C 0 (5129 ± 757 ng/mL) and AUC 0-t (7858 ± 1307 ng h/mL) of CPT-11 in the CPT-11 single administration group, the C 0 (4574 ± 371 ng/mL) and AUC 0-t (8779 ± 601 ng h/mL) after the separated co-administration remained unchanged, but the pre-mixed co-administration resulted with a significant increased C 0 (29,454 ± 12,080 ng/mL) and AUC 0-t (15,539 ± 5165 ng h/mL) (p < 0.05). Since the exposures of CPT-11 in most tissues in the pre-mixed co-administration group were dramatically lower than the separated co-administration group, the increased CPT-11 plasma concentration may be produced by the delayed tissue distribution because of the encapsulation by the components contained in KA injection, such as polysaccharides. Similar differences were also found in its metabolite, SN-38 G. There are obvious herb-drug interactions between CPT-11 injection and KA injection after the pre-mixed co-administration. The resulting excessive CPT-11 in the plasma may lead to many serious ADRs. Therefore, the full evaluation of herb-drug interactions is necessary and inappropriate combinations should be avoided.
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PREPARATIVE BIOCHEMISTRY & BIOTECHNOLOGY
·
2019
·
IF 1.117
Leilei Zhao,Qiong Jiang,Sitong Luo,Jie Shen,Xinjun Xu
Hepatic stimulator substance (HSS) is prepared by the freeze–thaw method on a large scale, but it is time-consuming and inefficient. It is necessary to find a better method to improve the efficiency and yield of HSS. In this study, HSS was prepared by enzymatic hydrolysis of neonatal porcine liver with trypsin, papain, dispase, and alcalase. Relatively, dispase was found to be the best enzyme, based on the results of the degree of hydrolysis and MTT assay. Box–Behnken design-response surface method was used to optimize the conditions, which were as follows: enzyme (dispase) concentration, 4164 U/g; substrate concentration, 7% (w/v); hydrolysis time, 4.3 hr; temperature, 45 °C; and pH, 6.5. The degree of hydrolysis was (54.99 ± 1.57)%. Shotgun proteomics coupled with Gene Ontology (GO) analysis based on the PANTHER classification system was used to screen proteins from neonatal porcine liver. The results profiled the proteins into biological processes, molecular functions, and cellular components, thus laying a foundation for further studies on components involved in and mechanisms of liver regeneration. Overall, the results suggest that enzymatic hydrolysis might be a promising method for industrial application.
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2019
·
IF 2.983
Xue-Mei Han,Yan-Jie Qin,Ying Zhu,Xin-Lin Zhang,Nan-Xi Wang,Ying Rang,Xue-Jia Zhai,Yong-Ning Lu
Sensitive and comprehensive measurement of systemic metabolites of tryptophan, phenylalanine and glutamate metabolism in biological samples is effective for understanding the pathogenesis of depression and other neurological diseases. Therefore, this study developed an underivatized liquid chromatography tandem mass spectrometry (LC–MS/MS) method for simultaneous monitoring the 3 components of glutamate metabolism in rat hippocampus and 11 components of tryptophan and phenylalanine metabolism in rat hippocampus, plasma and urine, and applied it to investigate their changes in rats induced by chronic unpredictable mild stress (CUMS). The investigated analytes are as follows: tryptophan, serotonin, 5-hydroxyindoleacetic acid, kynurenine, kynurenic acid, xanthurenic acid, 3-hydroxyanthranilic acid, quinolinic acid, phenylalanine, tyrosine, tyramine, glutamate, glutamine and gamma-aminobutyric acid. The method was verified to be sensitive and effective with satisfactory linearity, accuracies in the range of 78.2%–120.4%, and precisions less than 17.8% for all identified analytes. A series of significant changes in CUMS-induced rats can be detected: tryptophan, serotonin and tyrosine levels decreased and quinolinic acid increased in both hippocampus and plasma. In addition, the kynurenine/tryptophan ratios increased in hippocampus and plasma, the kynurenic acid/quinolinic acid ratios of plasma and urine were significantly reduced. These findings demonstrated that the CUMS procedure could lead to the central and peripheral imbalances of tryptophan and phenylalanine metabolism. In conclusion, a LC–MS/MS method for simultaneous measurement of several neurotransmitters in rat hippocampus, plasma and urine was developed and successfully applied to investigation of the central and peripheral changes in CUMS-induced rats. The method would be expected to provide applicability to the study of the mechanisms of depression and other related diseases associated with these neurotransmitters.
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JOURNAL OF SEPARATION SCIENCE
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2019
·Vol. 43
·期 3
·590-597
·
IF 2.516
Hong Pan,Feng Yang,Daiyuan Xiang,Fuguo Shi
Xanthii Fructus is extensively used as an herbal medicine. Ingestion of this herb is associated with severe hepatotoxicity and nephrotoxicity. Atractyloside and carboxyatractyloside are two dominative toxic constituents in Xanthii Fructus. However, their pharmacokinetic study is lacking. In this study, a novel high-performance liquid chromatography-tandem mass spectrometry method was developed to simultaneously quantify the rat plasma concentrations of atractyloside and carboxyatractyloside. After protein precipitation, the analytes were chromatographic separated on a ZORBAX Eclipse Plus column (2.1 × 150 mm id, 5 µm) under gradient elute. In the negative electrospray ionization mode, the transitions at m/z 725.3→645.4 for atractyloside, m/z 769.3→689.4 for carboxyatractyloside, and m/z 479.2→121.1 for paeoniflorin (the internal standard) were acquired by multiple reaction monitoring. This analytical method showed good linearity over 1–500 ng/mL for atractyloside and 2–500 ng/mL for carboxyatractyloside with acceptable precision and accuracy. No matrix effect, instability and carryover occurred in the analysis procedure. The extraction recoveries were greater than 85.0%. This method was applied to a preliminary pharmacokinetic study by orally administering Xanthii Fructus extract (9 g/kg) to rats, which was useful to evaluate the role of these two compounds in Xanthii Fructus-induced toxicity.
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JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
·
2015
·
IF 2.912
Xin Li,Man-Man Wang,Guo-Ying Zheng,Lian-Feng Ai,Xue-Sheng Wang
A hydrophobic monolith (10 mm × 2.1 mm i.d.) was developed as a reusable online solid-phase extraction (SPE) sorbent coupled with LC-MS/MS for the rapid determination of five avermectin residues in foodstuffs of both plant and animal origin. The online SPE was achieved using a 10 mmol/L ammonium acetate solution as the loading solvent, and acetonitrile (MeCN) was selected for the washing step. After being transferred from the monolith into a C18 analytical column using MeCN, the analytes were analyzed by LC-MS/MS using MeCN/0.1% NH4OH (10:90, v/v) as the mobile phase. The detection limit was 2 μg/kg for five avermectins, and the recoveries in fresh pear, chili seed, bovine muscle, and milk ranged from 71.8% to 101.3% with relative standard deviations of less than 8.94%. The online SPE and determination were achieved within 15 min, and the monolithic extractor was reusable for more than 500 experiments.
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BIOMEDICAL CHROMATOGRAPHY
·
2015
·Vol. 29
·期 11
·1737-1743
·
IF 1.723
Xue-jia Zhai,Fen Chen,Chao-ran Zhu,Yong-ning Lu
Many amino acid neurotransmitters in urine are associated with chronic stress as well as major depressive disorders. To better understand depression, an analytical LC-MS/MS method for the simultaneous determination of 11 underivatized neurotransmitters (4-aminohippurate, 5-HIAA, glutamate, glutamine, hippurate, pimelate, proline, tryptophan, tyramine, tyrosine and valine) in a single analytical run was developed. The advantage of this method is the simple preparation in that there is no need to deconjugate the urine samples. The quantification range was 25–12,800 ng mL −1 with >85.8% recovery for all analytes. The nocturnal urine concentrations of the 11 neurotransmitters in chronic unpredictable mild stress (CUMS) model rats and control group ( n = 12) were analyzed. A series of significant changes in urinary excretion of neurotransmitters could be detected: the urinary glutamate, glutamine, hippurate and tyramine concentrations were significantly lower in the CUMS group. In addition, the urinary concentrations of tryptophan as well as tyrosine were significantly higher in chronically stressed rats. This method allows the assessment of the neurotransmitters associated with CUMS in rat urine in a single analytical run, making it suitable for implementation as a routine technique in depression research. Copyright © 2015 John Wiley & Sons, Ltd.
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2014
·
IF 2.694
Zhiyong Zhao,Qinxiong Rao,Suquan Song,Na Liu,Zheng Han,Jiafa Hou,Aibo Wu
A simple and reliable method for simultaneous determination of deoxynivalenol-3-glucoside and major type B trichothecenes (deoxynivalenol, nivalenol, fusarenon X, 3-acetyldeoxynivalenol, 15-acetyldeoxynivalenol and deepoxy-deoxynivalenol) in animal feed and raw materials has been developed and validated in this study. The method was based on an improved dispersive solid-phase extraction (DSPE) followed by analysis using high performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS). Also, matrix-matched calibration curve ( R 2 > 0.99) was employed to minimize matrix effects and ensure accurate quantification. The recoveries during sample preparation process (including extraction and clean-up) ranged from 79.03% to 118.39%, with intra-day and inter-day relative standard deviation lower than 20% for all the analytes. The limit of quantification ranged from 5.0 μg/kg for deoxynivalenol to 13.6 μg/kg for fusarenon X. The validated method was successfully applied to the analysis of animal feed and corn. The pilot study showed that 37 out of 41 samples were contaminated with deoxynivalenol-3-glucoside at the levels of 6.0–121.0 μg/kg. Most of the type B trichothecenes were also found with the exception of fusarenon X, at the contaminated levels of 10.0–1382 μg/kg. To the best of our knowledge, this was the first scientific report on the co-occurrence of masked deoxynivalenol and type B trichothecenes in animal feed and raw materials.
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