BIOMEDICAL CHROMATOGRAPHY
·
2024
·Vol. 38
·期 11
·e6011
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IF 1.8
Kejun Zhang,Haizhou Wang
Huperzine A is a reversible and selective cholinesterase inhibitor and has been approved for the treatment of Alzheimer's diseases. In this study, we developed a highly sensitive and specific ulta-high-performance liquid chromatography–tandem mass spectrometry method for the determination of Huperzine A in rat plasma. An aliquot of 50 μL of rat plasma sample was pretreated with 200 μL of acetonitrile-methanol ( v/v ; 1:1) containing 0.2% formic acid followed by solid phase extraction. The resulting sample was separated on a Waters ACQUITY BEH C 18 column using acetonitrile and water containing 0.2% formic acid as mobile phase, at a flow rate of 0.3 mL/min. Multiple-reaction monitoring (MRM) mode was used for quantitative analysis of Huperzine A in positive electrospray ionization. In the concentration range of 0.01–10 ng/mL, Huperzine A showed excellent linearity with correlation coefficient > 0.998. The intra- and inter-day RSD% were less than 9.7%, while the RE% ranged from −6.7% to 10.0%. The mean recovery was >84.5%. The validated method was demonstrated to be selective, sensitive, and reliable, which has been successfully applied to pharmacokinetic study of Huperzine A in rat plasma. Huperzine A displayed a long half-life in rat plasma and high oral bioavailability.
研究领域:
分析化学
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药理学
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神经科学
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PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2024
·
IF 4.9
Tingting Fan,Xiangwei He,Hengchao E,Yanmei Zhang,Xiaobei Li,Xujiao Li,Xianli Yang,Changyan Zhou,Zhiyong Zhao,Xiaoyan Zhao
Gyromitrin is the main toxic metabolite produced from the false morel such as Gyromitra esculenta , which has a long history of causing food poisoning. However, how to identify the gyromitrin-induced poisoning is difficult because the biomarker of gyromitrin in vivo is still unclear. In this study, a novel isotope-coded method combined with the derivatization strategy was first developed for the accurate quantification of gyromitrin in urine and plasma by ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). The major parameters affecting the derivatization efficiency were systematically investigated, and the p-tolualdehyde-d 4 was employed to form the isotope internal standard. The developed method was fully validated with the limit of detection (LOD) of 1 µg/L in urine and plasma. The recoveries were between 88 % and 111 % with the inter-day precision less than 13 %. An exposure study in 12 rats was conducted to determine urinary excretion of gyromitrin and its metabolite monomethylhydrazine (MMH). The mean urinary excretion rates of gyromitrin were 3.45 % (low dose) and 4.93 % (high dose), while the excretion rate of MMH were 0.20 % and 0.36 %. After exposure for 48 h, no gyromitrin and MMH was detected in rat urine. The results suggested that gyromitrin is a valuable biomarker for identification of gyromitrin-induced mushroom poisoning.
研究领域:
毒理学
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分析化学
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食品安全
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高影响因子
Metabolites
·
2022
·Vol. 12
·期 9
·790
·
IF 5.581
Chengcai Zhang,Yang Jiang,Changzheng Liu,Linyuan Shi,Jintong Li,Yan Zeng,Lanping Guo,Sheng Wang
Fagopyrum dibotrys, being native to southwest China, is widely distributed in Yunnan, Guizhou Provinces and Chongqing City. However, the quality of medicinal materials growing in different origins varies greatly, and cannot meet the market demand for high-qualityF. dibotrys. In this study, 648 metabolites were identified, and phenolic compounds ofF. dibotrysfrom different origins were clearly separated by principal component analysis (PCA). Our results suggested that the medicinal differences ofF. dibotrysfrom different origins can be elucidated via the variations in the abundance of the phenolic and flavonoid compounds. We found that the epicatechin, total flavonoids and total tannin content in Yunnan Qujing (YQ) and Yunnan Kunming (YK) were higher than those in Chongqing Shizhu (CS), Chongqing Fuling (CF) and Guizhou Bijie (GB), suggesting that Yunnan Province can be considered as one of the areas that produce high-quality medicinal materials. Additionally, 1,6-di-O-galloyl-β-D-glucose, 2,3-di-O-galloyl-D-glucose and gallic acid could be used as ideal marker compounds for the quality control ofF. dibotrysfrom different origins caused by metabolites, and theF. dibotrysplanted in Yunnan Province is well worth exploiting.
研究领域:
植物学
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药理学
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分析化学
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DOI
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2022
·
IF 3.571
Mingxin Dai,Qian Wang,Shanshan Kou,Xinyu Li,Zhenzhou Jiang,Lixin Sun,Xin Huang
Tryptophan (TRP) metabolism plays a crucial role in pathology and physiology. An imbalance in TRP metabolism has been implicated in the pathology of renal failure. To explore the changes in the TRP profile that occurred in renal failure, we induced experimental models of renal ischemia-reperfusion injury (RIRI) and chronic renal failure (CRF) in rats. A simple, rapid and sensitive method coupling ultra-high-performance liquid chromatography to triple quadrupole mass spectrometry (UPLC-MS/MS) was developed for the simultaneous determination of TRP and its seven major metabolites in plasma. The method was validated base on linearity, accuracy, precision, stability, recovery and the matrix effect. In the RIRI group, the levels of kynurenine (KYN), 5-hydroxyindoleacetic acid (5-HIAA), tryptamine (Trpm) and kynurenic acid (KA) were increased, and the level of TRP was decreased significantly compared with those of sham group. Moreover, the levels of most of the metabolites measured using the proposed method changed significantly with CRF progression. In the CRF group, the levels of KYN, 5-HIAA, Trpm, KA, 3-hydroxyanthranilic acid (3-HAA) and 3-hydroxykynurenine (3-HK) were dramatically elevated, and the level of TRP was markedly reduced compared with those of the CON group. Plasma precursor metabolite/product metabolite ratios were calculated to characterize enzyme activity . Principal component analysis (PCA) and orthogonal partial least squares discriminant analysis (OPLS-DA) of the metabolites were performed for both groups. A Spearman correlation coefficient analysis between the metabolite concentrations and renal injury indicators was performed. We identified KYN, TRP, and 5-HIAA as potential metabolite biomarkers for AKI , and 5-HIAA, TRP, 3-HAA, KA, KYN and 3-HK as potential metabolite biomarkers for CRF (VIP>1 and p < 0.05). These results showed significant changes in the tryptophan metabolism profile under the two types of renal failure. In summary, the results of our study depict the changes in the TRP pathway, reveal the role of the TRP pathway in AKI and CRF, and provide insight into finding potential peripheral biomarkers of renal failure and elucidating the mechanism of diseases related to TRP metabolism disorders .
研究领域:
药理学
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生物化学
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肾病学
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代谢组学
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DOI
PubMed
高影响因子
ANALYST
·
2024
·
IF 3.6
Yinan Zhang,Guanghui Wang,Yongjian Shao,Pei Zheng,Chunyan Guo,Zhiqun Liu,Lilai Shen,Zhiquan Liu,Jiafeng Ding,Hangjun Zhang
To objectively quantify changes in steroid hormones in organisms caused by adverse environmental loads, we developed a simple and sensitive UPLC–MS/MS (ultra-performance liquid chromatography triple quadrupole mass spectrometry) method for the simultaneous determination of 18 steroid hormones on the HPG axis. This analytical method based on liquid extraction and a multimode electrospray and at-mospheric pressure chemical ionization (ESCi) source, which was optimized by mass spectrometry, liquid phase and pretreatment for the quantification of choles-terol [CH], aldosterone [A], cortisone [E], hydrocortisone [F], 21-deoxycortisol [21-DF], corticosterone [B], 11-deoxycortisol [11-DF], androstenedione [A2], estradiol [E2], estrone [E1], 2-methoxyestradiol [2-MeE2], 21-hydroxyprogesterone [21-OHP], 17-α hydroxyprogesterone [17α-OHP], testosterone [T], dehydroepiandrosterone [DHEA], progesterone [P4], dihydrotestosterone [DHT], and pregnenolone [P5]. The method exhibits linearity in the analyte-concentration range 0.03–1000 μg/mL range (r2 > 0.99), spiked recoveries for the concentration range tested are 76.22%–113.66%, and the relevant parameters of precision are 7.52%–1.14%. Compared to other method, this new method not only uses a small amount of serum (only 100 μL), but also permitted the analysis of the challenging steroids, cholesterol. Furthermore, the method was successfully applied to determination of steroids in Mus musculus, Carassius auratus, Rana catesbiana Shaw, and Rana nigromaculata serum samples from randomly selected individuals. This method may therefore be very useful tool as an efficient analysis method for assessing changes in steroid hormones.
研究领域:
分析化学
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内分泌学
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环境科学
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PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2024
·
IF 3.1
Hongjian Kang,Jixia Wang,Yanfang Liu,Feifei Huang,Han Zhou,Xiaomin Xie,Qing Xu,Xinmiao Liang,Xingya Xue
Traditional Chinese medicines (TCMs) are popular in clinic because of their safety and efficacy. They contain abundant natural active compounds, which are important sources of new drug discovery. However, how to efficiently identify active compounds from complex ingredients remains a challenge. In this study, a method combining UHPLC-MS/MS characterization and in silico screening was developed to discover compounds with dopamine D2 receptor (D2R) activity in Stephania epigaea ( S. epigaea ). By combining the compounds identified in S. epigaea by UHPLC-MS/MS with reported compounds, a virtual library of 80 compounds was constructed for in silico screening. Potentially active compounds were chosen based on screening scores and subsequently tested for in vitro activity on a transfected cell line CHO-K1-D2 model using label-free cellular phenotypic assay. Three D2R agonists and five D2R antagonists were identified. (-)-Asimilobine, N -nornuciferine and (-)-roemerine were reported for the first time as D2R agonists, with EC 50 values of 0.35 ± 0.04 μM, 1.37 ± 0.10 μM and 0.82 ± 0.22 μM, respectively. Their target specificity was validated by desensitization and antagonism assay. (-)-Isocorypalmine, (-)-tetrahydropalmatine, (-)-discretine, (+)-corydaline and (-)-roemeroline showed strong antagonistic activity on D2R with IC 50 values of 92 ± 9.9 nM, 1.73 ± 0.13 μM, 0.34 ± 0.02 μM, 2.09 ± 0.22 μM and 0.85 ± 0.08 μM, respectively. Their kinetic binding profiles were characterized using co-stimulation assay and they were both D2R competitive antagonists. We docked these ligands with human D2R crystal structure and analyzed the structure-activity relationship of aporphine-type D2R agonists and protoberberine-type D2R antagonists. These results would help to elucidate the mechanism of action of S. epigaea for its analgesic and sedative efficacy and benefit for D2R drug design. This study demonstrated the potential of integrating UHPLC-MS/MS with in silico and in vitro screening for accelerating the discovery of active compounds from TCMs.
研究领域:
药理学
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生物信息学
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中药学
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DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2024
·
IF 8.5
Yan Qi,Chuwen Mao,Yanru Zhou,Zuohua Xie,Chao Wu,Songyi Lin
This paper employed a physiologically based pharmacokinetic model (PBPK) to investigate the transformations of folic acid and its metabolites in vivo. Additionally, an ultra-performance liquid chromatography (UPLC) method was developed to accurately measure the body's retention rate and conversion rate of folic acid, tetrahydrofolate, and 5-methyltetrahydrofolate. Furthermore, the bioavailability of folic acid in the body was assessed by combining this method with an evaluation technique for animal models. The study found that the gastric metabolism time was 2 h, while the small intestinal metabolism duration was 4 h. The maximum conversion rate was observed in plasma and liver after 6 h, and in the brain after 8 h. This serves as a framework for creating a model to assess the bioavailability of folic acid in living organisms, to enhance the safety and efficacy of folic acid intake.
研究领域:
药理学
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分析化学
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生物医学工程
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PubMed
高影响因子
RSC Advances
·
2026
·Vol. 16
·期 9
·8278-8288
·
IF 6.1
Ajiao Hou,Chao Yu,Jinbo Li,Liu Yang,Haixue Kuang,Yanyan Zhou,Hai Jiang
In the Chinese Pharmacopoeia (2025 Edition), it is reported that Siegesbeckiae herba (SH) can be processed via a single herb preparation, demonstrating significant economic value and development potential. However, the quality evaluation of its processed products mostly relies on personal experience, which severely restricts the trade and circulation of SH. This study aimed to explore the correlation between different processing methods and the appearance color of SH, simplify the quality evaluation process, and improve the accuracy of sensory evaluation. Firstly, a colorimeter was used to quantify the appearance color of SH processed by different methods, UPLC-QDA was employed to establish the fingerprint of SH under different processing methods, and pharmacodynamic experiments were conducted to determine its analgesic and anti-inflammatory activities. Subsequently, chemometrics was applied to analyze the correlation between different processing methods and the appearance color of SH, thereby optimizing the optimal processing technology of SH. Finally, osteoarthritis experiments were performed to further verify the results. The colorimeter, fingerprint analysis, and pharmacodynamic results all confirmed that the SH steamed repeatedly for nine times exhibited a shiny black color and the best efficacy. This study provides a reference for the color evaluation of the processing standard of SH and the standardization of the macroscopic characteristics of traditional Chinese medicine.
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PubMed
高影响因子
FOOD CHEMISTRY
·
2026
·
IF 10.4
Rong Bao,Rongting Zhuo,Zhuxiang Zhong,Yan Yang
Antibiotic residues in animal-derived foods raise food safety concerns. This study developed a QuEChERS–UPLC–MS/MS method for the simultaneous detection of multiple antibiotics in animal-derived foods. Key QuEChERS pretreatment parameters were systematically optimized using response surface methodology with a central composite design to identify the optimal extraction solvents, salting-out agents, and clean-up sorbents. Method validation met the requirements of European Commission Implementing Regulation (EU) 2021/808, confirming suitability for rapid determination of 85 antibiotics across diverse food matrices. Analysis of 590 samples detected antibiotic residues in 39.8% of samples, representing 36 different antibiotics. Health risk assessment showed a Hazard Index (HI) < 1, indicating low risk at current consumption levels for the local population. Nevertheless, this high detection frequency highlights the need for continued monitoring of antibiotic residues in animal-derived foods.
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PubMed
高影响因子
Food Chemistry-X
·
2026
·
IF 9.2
Changdong Lin,Juyuan Luo,Shuo Wang,Cheng Shen,Shucan Zhang,Yongling Liu,Zhibo Song,Yumei Ma,Tao Chen,Yulin Li
Affinity ultrafiltration is widely used for rapid, targeted screening of bioactive natural compounds, but high-abundance components in complex matrices often mask low-abundance yet potent inhibitors, reducing sensitivity. Here, barley seedling extracts were preprocessed via HPLC peak-area clustering before affinity ultrafiltration to identify α-glucosidase inhibitors. This “clustering-prior-to-ultrafiltration” strategy enabled the discovery of four additional low-abundance inhibitors overlooked by direct ultrafiltration. These compounds exhibited stronger inhibitory activity (IC 50 : 217.75–583.35 μg/mL) than the three high-abundance components (IC 50 : 707.05–1044.95 μg/mL). Enzyme kinetics, spectroscopy, molecular docking, and dynamic simulations revealed their binding mechanisms. This approach enhances screening sensitivity and provides a basis for developing functional foods.
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PubMed
高影响因子
Arabian Journal of Chemistry
·
2024
·
IF 5.3
Yuyi Liu,Xuan Hu,Enhui Li,Yajing Fang,Hui Xue,Jiachao Zhang,Rajesh Jha,Ruimin Wang
Paederia foetida L. leaf (PFL) is recognized for its uric acid-lowering. However, the key compounds and their mechanisms of countering hyperuricemia remain unclear. In this study, bioaffinity ultrafiltration in combination with UPLC-ESI-QTrap-MS/MS was used to screen and identify potential xanthine oxidase (XO) inhibitors in the purified PFL extract, and the possible mechanisms of their interaction were investigated by molecular docking. The experimental results showed that the purified PFL extract exhibited excellent antioxidant and anti-XO effect. Further the results of enzyme inhibition experiments in vitro showed that luteolin-7- O -glucoside (IC 50 = 61.41 μg/mL), astragalin (IC 50 = 114.89 μg/mL), quercitrin (IC 50 = 124.50 μg/mL), dihydromyricetin (IC 50 = 296.32 μg/mL), cyanidin-3- O -rutinoside (IC 50 = 373.82 μg/mL), kaempferol-3- O -rutinoside (IC 50 = 450.10 μg/mL) and (-)-epigallocatechin (IC 50 = 610.48 μg/mL) in purified PFL extract were the major contributors to the XO inhibitory activity, and confirmed this finding. Molecular docking revealed these inhibitors interact with critical XO residues through hydrogen bonding, hydrophobic, and electrostatic interactions, highlighting flavonoids in purified PFL extract as potent XO inhibitors. This work provides insight into flavonoids in the purified PFL extract as potent XO inhibitors.
研究领域:
药理学
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生物化学
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分析化学
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DOI
高影响因子
MICROCHIMICA ACTA
·
2025
·Vol. 192
·期 11
·1-18
·
IF 5.3
Xie Kexin,Wang Chunfeng,Pang Ningjia,Cheng Yanan,Chen Mengyi,Mu Taotao,Xiao Deli,Di Bin
The design and synthesis of Fe 3 O 4 @PDA@poly(AA-co-EGDMA) nanoparticles (NPs) as a novel magnetic solid-phase extraction (MSPE) material for efficient enrichment and detection of synthetic cannabinoids (SCs) of various structures in large-volume wastewater is reported. The Fe 3 O 4 @PDA@poly(AA-co-EGDMA) NPs were synthesized via a two-step process involving dopamine polymerization and functionalization with poly(acrylic acid-co-ethylene glycol dimethacrylate) polymers, providing hydrophobic and acidic functional groups for enhanced analyte adsorption. An MSPE-ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed and optimized for the detection of 24 SCs in wastewater. The method exhibited excellent analytical performance with good linearity ( R > 0.99), low limits of quantification (LOQ, 0.02–0.1 ng/L), and good precision with recoveries ranging from 50.20 to 92.72%. The method is capable of reliably analyzing trace SCs in large volume samples (300 mL and 1 L). This study introduces a simple, rapid, and cost-effective MSPE-UPLC-MS/MS approach for detecting SCs in complex environmental samples. The proposed method offers significant potential for wastewater-based epidemiology (WBE) applications, providing a valuable tool for monitoring drug use trends, public health surveillance, and regulatory enforcement. Graphical
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