MICROCHEMICAL JOURNAL
·
2024
·
IF 4.9
Weihao Ma,Hao Zhang,Jiayuan Nie,Chunyu Qiang,Zhiwei Li,Ling Ma,Ke Wang
In this study, a novel magnetic covalent organic framework (Fe 3 O 4 @SiO 2 -HBTA-TTA-COF) was synthesized, which was fully characterized by scanning electron microscopy, transmission electron microscopy, etc. Furthermore, a new method was developed for the determination of 25 quinolones (QNs) in water and milk using the Fe 3 O 4 @SiO 2 -HBTA-TTA-COF as magnetic solid-phase extraction adsorbent coupled with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Meanwhile, various experimental parameters were optimized including sample solution pH, adsorbent dosage and extraction time, etc. Under the optimal conditions, good linearity in the range of 0.1–200 μg·L −1 (R 2 ≥ 0.999) were obtained, the recoveries of 25 QNs were 70.04 %–104.4 % with the relative standard deviations lower than 9.87 % (n = 5), the limits of detection were 0.003–0.010 μg·L −1 for water and 0.018–0.722 μg·kg −1 for milk. This established method was high-sensitive and high-throughput, which can be used as a good alternative method for the selective determination of 25 QNs in water and milk.
研究领域:
分析化学
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环境科学
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食品科学
✓ 已验证
产品关联
DOI
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2025
·
IF 3.8
Jiang Haipeng,Xu Wenxi,Bi Tian,Wang Biao,Shi Mengyun,Lv Jiamin,Liu Huwei
Screening of ligands from natural products, especially traditional herbs, has always been an important pathway for drug discovery. In the current work, we present a strategy for the screening of active substances from TCM by combination of in silico target prediction, surface plasmon resonance (SPR), and UPLC-HR-MS/MS, using Kansui as an illustration. In the first, in silico target prediction of diterpenoids from Kansui was performed, aiming to improve the success rate of screening. Carbonic anhydrase II (CA II) were within the most likely targets. Then, SPR combined with UPLC-HR-MS/MS analysis was employed for the screening of ligands for CA II from a mixture of Kansui extract and for the structural identification of the captured ingredients. It was found that the ligands of CA II are mainly ingenane-type diterpenoids, which was further validated by enzymatic activity experiments and molecular docking that ingenane-type diterpenoids have more affinity and potency for CA II activation. It is the first time that the ligands of CA II have been screened from the extract of K ansui, and the present ligand screening work also providing clues to the pharmacological mechanisms and rationality of vinegar-processed Kansui . Graphical
研究领域:
中药学
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药物化学
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生物信息学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF ETHNOPHARMACOLOGY
·
2023
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IF 5.4
Yudan Mei,Xiaoyu Tong,Yumei Hu,Wenjun Liu,Jiajia Wang,Kaihong Lv,Xu Li,Liang Cao,Zhenzhong Wang,Wei Xiao,Xia Gao
Ethnopharmacological relevance Shen-Wu-Yi-Shen tablets (SWYST), a Chinese patent medicine consisting of 12 herbal medicines, was formulated by a famous TCM nephrologist, Zou Yunxiang. It is clinically used to improve the symptoms of nausea, vomiting, poor appetite, dry mouth and throat, and dry stool in patients with chronic renal failure (CRF) accompanied by qi and yin deficiency, dampness, and turbidity. SWYST can reduce urea nitrogen, blood creatinine, and urinary protein loss, and increase the endogenous creatinine clearance rate. However, little is known about its pharmacokinetics . Aim of study To compare the pharmacokinetics of six bioactive components after oral administration of SWYST in normal and adenine-induced CRF rats. Materials and methods A method based on ultra-performance liquid chromatography coupled with a triple-stage quadrupole mass spectrometer (UPLC-TSQ-MS/MS) was developed and validated to determine the six bioactive compounds (albiflorin, paeoniflorin , plantagoguanidinic acid, rhein , aloe-emodin, and emodin) in rat plasma. Rat plasma samples were prepared using protein precipitation. Chromatography was performed on an Agilent Eclipse Plus C 18 column (3.0 × 50 mm, 1.8 μm) using gradient elution with a mobile phase composed of acetonitrile and water containing 0.1% (v/v) formic acid, while detection was achieved by electrospray ionization MS under the multiple selective reaction monitoring modes. After SWYST administration, rat plasma was collected at different time points, and the pharmacokinetic parameters of six analytes were calculated and analyzed based on the measured plasma concentrations. Results The UPLC-TSQ-MS/MS method was fully validated for its satisfactory linearity ( r ≥ 0.9913), good precisions (RSD <11.5%), and accuracy (RE: -13.4∼13.1%), as well as acceptable limits in the extraction recoveries, matrix effects, and stability (RSD <15%). In normal rats, the six analytes were rapidly absorbed (T max ≤ 2 h), and approximately 80% of their total exposure was eliminated within 10 h. Moreover, in normal rats, the AUC 0-t and C max of albiflorin , plantagoguanidinic acid, and rhein exhibited linear pharmacokinetics within the dose ranges, while that of paeoniflorin is non-linear. However, in CRF rats, the six analytes exhibited reduced elimination and significantly different AUC or C max values. These changes may reflect a decreased renal clearance rate or inhibition of drug-metabolizing enzymes and transporters in the liver and gastrointestinal tract caused by CRF. Conclusions A sensitive UPLC-TSQ-MS/MS method was validated and used to investigate the pharmacokinetics of SWYST in normal and CRF rats. This is the first study to investigate the pharmacokinetics of SWYST, and our findings elucidate the causes of their different pharmacokinetic behaviors in CRF rats. Furthermore, the results provide useful information to guide further research on the pharmacokinetic-pharmacodynamic correlation and clinical application of SWYST.
研究领域:
民族药理学
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药代动力学
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中药学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2015
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IF 2.979
Min Liao,Cong Dai,Mengping Liu,Jiefeng Chen,Zuanguang Chen,Zhiyong Xie,Meicun Yao
A novel, sensitive and rapid ultra-performance liquid chromatography–tandem mass spectrometric (UPLC–MS/MS) method for simultaneous quantification of four furostanol glycosides in rat plasma was established and validated. Ginsenoside Rb1 was used as an internal standard. Plasma samples were pretreated by liquid–liquid extraction with n -butanol and chromatographed on a C18 column (2.1 × 50 mm i.d., 2.6 μm) using a gradient elution program consisting of acetonitrile and water (containing 0.03% formic acid and 0.1 mM lithium acetate) at a flow rate of 0.4 mL/min. Lithium adduct ions were employed to enhance the response of the analytes in electrospray positive ionization mode and multiple reaction monitoring transitions were performed for detection. All calibration curves exhibited good linearity ( r > 0.999) over the range of 10–20,000 ng/mL for protodioscin and 2–4000 ng/mL for protogracillin, pseudoprotodioscin and pseudoprotogracillin. The recoveries of the whole analytes were more than 80.3% and exhibited no severe matrix effect. Meanwhile, the intra- and inter-day precisions were all less than 10.7% and accuracies were within the range of −8.1–12.9%. The four saponins showed rapid excretion and relative high plasma concentrations when the validated method was applied to the PK study of Dioscorea nipponica extracts by intragastric administration at low, medium and high dose to rats. Moreover, the T 1/2 and AUC 0– t of each compound turned out to behave in a dose-dependent pattern by comparing them at different dose levels.
研究领域:
分析化学
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药理学
✓ 已验证
DOI
PubMed
高影响因子
TALANTA
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2016
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IF 4.035
Xinpeng Dai,Xiuna Jia,Pan Zhao,Ting Wang,Jian Wang,Peiting Huang,Lu He,Xiaohong Hou
As a novel kind of materials, metal-organic frameworks (MOFs) have great potential for the preconcentration of trace analytes. In our work, MIL-101(Cr) was prepared and applied as a solid phase extraction (SPE) sorbent for the pretreatment of sulfadiazine (SDA), sulfamethazine (SMZ), sulfachloropyridazine (SCP) and sulfamethoxazole (SMX) in different environmental water samples coupling with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) detection. Experimental parameters, such as SPE materials, pH of water sample, volume of sample, flow rate , and type and volume of elution solvent, were properly optimized. Under the optimum conditions, good sensitivity levels were achieved with the detection limits of 0.03–0.08 μg/L and the quantitation limits of 0.11–0.27 μg/L. The linear ranges were from 0.2–40 or 0.5–100 μg/L ( r 2 >0.996) for the analytes, and the relative recoveries were in the range from 83.5% to 107.3% with the relative standard deviations (RSD) between 0.2% and 8.0% ( n =6). In addition, computational simulation was primarily used to predict the adsorption of MIL-101(Cr) toward sulphonamides (SAs), and also demonstrated the molecular interactions and free binding energies with the molecular modeling method. The results revealed that the combination of experimental and computational study not only accurately recognized the adsorption of MIL-101(Cr) on SAs, but also provided a new strategy on the trace contaminant analysis.
研究领域:
环境科学
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分析化学
✓ 已验证
DOI
高影响因子
FOOD CHEMISTRY
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2013
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IF 3.334
Guisheng Zhou,Hanqing Pang,Yuping Tang,Xin Yao,Yunhe Ding,Shaoqing Zhu,Sheng Guo,Dawei Qian,Juan Shen,Yefei Qian,Shulan Su,Li Zhang,Chun Jin,Yong Qin,Jin-Ao Duan
In this study, a rapid, simple and sensitive analytical method was developed for the quantitative determination of 20 nucleosides and nucleobases in functional foods at trace levels using hydrophilic interaction ultra-performance liquid chromatography coupled with triple-quadrupole tandem mass spectrometry (HILIC-UPLC–TQ-MS/MS) in multiple-reaction monitoring (MRM) mode. Under optimised chromatographic conditions, good separation of 20 target compounds was achieved using a Waters Acquity UPLC BEH Amide column and gradient elution in 11 min. The limits of detection (LODs) and quantification (LOQs) were between 0.02–42.54 ng/mL and 0.05–98.18 ng/mL for the 20 analytes, respectively. This is the first report about simultaneous analysis of nucleosides and nucleobases in functional foods using this method, which afforded good linearity, precision, repeatability and accuracy. The method developed was successfully applied to quantify target compounds in batches of ginkgo seeds. The method potentially could be used to determine polar and trace-level nucleosides and nucleobases in ginkgo seeds.
研究领域:
分析化学
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食品科学
✓ 已验证
DOI
高影响因子
Arabian Journal of Chemistry
·
2021
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IF 5.165
Weizhuo Tang,Shuang Li,Miaomiao Wang,Bin Wang
In this study, simultaneous optimization of ultrasound-assistant extraction (UAE) of four representative groups of Osmanthus fragrans (OF) fruit was firstly performed using the response surface methodology (RSM). Subsequently, qualitative and quantitative analysis of irioid glycosides from the optimized OF fruit extract was performed using UPLC-ESI-Orbitrap-MS/MS. A total of 13 irioid glycosides were tentatively identified, of which six compounds were identified for the first time. Finally, the anti-inflammatory activity of the optimized OF var. aurantiacus Makino (OFA) fruit extract was evaluated based on a CuSO 4 -induced zebra fish model. The biological results demonstrated that OFA fruit extract at a concentration of 5 μg/mL could significantly reduce the number of macrophages, but no significant activities were observed at high concentrations (10 and 50 μg/mL). These results suggest that OF fruit has the promise as a functional additive in food for health promotion.
研究领域:
药理学
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分析化学
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食品科学
✓ 已验证
产品关联
DOI
高影响因子
Frontiers in Pharmacology
·
2021
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IF 5.811
Lan Zhenwei,Zhang Ying,Sun Yue,Wang Lvhong,Huang Yuting,Cao Hui,Wang Shumei,Meng Jiang
Recent studies concerning products that originate from natural plants have sought to clarify active ingredients, which both explains the mechanisms of the function and aids in quality control during production. As a traditional functional plant, Curcumae Rhizoma (CR) has been proven to be effective in promoting blood circulation and removing blood stasis. However, the components that play a role in its huge compound library are still unclear. The present study aimed to develop a high-throughput screening method to identify thrombin inhibitors in CR and validate them by in vitro and in vivo experiments. The effect of CR on thrombin in HUVECs cells was determined by ELISA, then an affinity-ultrafiltration-UPLC-Q-Exactive Orbitrap/MS approach was applied. Agatroban and adenosine were used as positive and negative drugs respectively to verify the reliability of the established method. The in vitro activity of the compounds was determined by specific substrate S-2238. The in vivo effect of the active ingredients was determined using zebrafish. Molecular docking was used to understand the internal interactions between compounds and enzymes. ELISA results showed that CR had an inhibitory effect on thrombin. The screening method established in this paper is reliable, by which a total of 15 active compounds were successfully identified. This study is the first to report that C7, 8, and 11 have in vitro thrombin-inhibitory activity and significantly inhibit thrombosis in zebrafish models at a safe dose. Molecular docking studies were employed to analyze the possible active binding sites, with the results suggesting that compound 16 is likely a better thrombin inhibitor compared with the other compounds. Based on the affinity-ultrafiltration-UPLC-Q-Exactive Orbitrap/MS approach, a precisely targeted therapy method using bio-active compounds from CR might be successfully established, which also provides a valuable reference for targeted therapy, mechanism exploration, and the quality control of traditional herbal medicine.
研究领域:
药理学
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生物化学
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中药学
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分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Analytical Methods
·
2025
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IF 2.6
Jieting Zhang,Shuo Diao,Zhen Huang,Mengyuan Wu,Xintong Wang,Yiran Zhao,Mingming Yu,Xianzhen Wang,Jingchun Yao,Guimin Zhang,Sherwin K. B. Sy,Zhihua Lv,Hai Yang
Guided by the principles of Analytical Quality by Design (AQbD), a highly selective and sensitive LC-MS/MS method was established for the simultaneous quantification of 15 compounds in Shouhui Tongbian capsules, enabling their effective quality control. The separation was carried out on a BEH C18 column (1.7 μm, 2.1 × 100 mm) with a mobile phase comprising 0.1% formic acid in 3 mM ammonium acetate aqueous solution and methanol (60 : 40, v/v) at a flow rate of 0.30 mL min−1. The method exhibited good linearity within a certain concentration range (R2 > 0.9906) depending on the compound; the precision ranged from 0.6% to 14.7% and accuracy was within 11.2%. Among the 15 detected compounds, aloin had the highest content in the Shouhui Tongbian capsules, reaching 227.3780 mg g−1, followed by betaine and L-hydroxyproline, with concentrations of 1.3204 mg g−1 and 1.2929 mg g−1, respectively. This method simultaneously detected the content of 15 compounds in five batches of Shouhui Tongbian capsules.
研究领域:
分析化学
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药物分析
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质量控制
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色谱-质谱分析
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中医药学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
ANALYTICA CHIMICA ACTA
·
2022
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IF 6.911
Lin Li,Hongyu Zhang,Mengdan Zhang,Ting Wang,Xiaohong Hou
MIL-88B(Fe)/cellulose microspheres (MIL-88B(Fe)/CMs) were characterized by the means of SEM, XRD, TGA and N 2 adsorption-desorption test. The composite was used as the sorbent for fully automated dispersive pipette extraction (DPX), after introducing CMs as the support, the loss of MIL-88B(Fe) in DPX was avoided. Coupled to UPLC-MS/MS, the proposed method was employed for the analysis of trace sulfonamides (SAs) in milk samples. The parameters affecting the extraction efficiency, including pH of sample solution, the rate of aspiration and dispense, amount of the adsorbent, type and volume of elution solvent were optimized. Under the optimal conditions, good linearity (r ≥ 0.9978 for five analytes), high sensitivity (limit of detection: 0.00660–0.0136 μg kg −1 ) and satisfactory recovery (69.8%–100.9%) were achieved. Furthermore, the sorbent showed desirable reusability over eight extraction cycles. Compared with other methods for the pretreatment of SAs, the proposed method showed advantages of high sensitivity, less sorbent consumption, environmental friendliness and automation, providing a promising protocol for sample preparation.
研究领域:
分析化学
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食品科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2021
·
IF 3.935
Menghua Zhang,Xiaoxue Liu,Zhiyao Chen,Shenhao Jiang,Lin Wang,Min Tao,Liyan Miao
Over the past decades, therapeutic drug monitoring (TDM) of tyrosine kinase inhibitors (TKIs) and their main active metabolites has shown benefits in improving treatment efficacy and safety. Therefore, a sensitive, simple and economical ultrahigh-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed and validated for the determination of six oral tyrosine kinase inhibitors (TKIs) and two active metabolites, including imatinib (IMA), N-desmethyl imatinib (NDIMA), sunitinib (SUNI), N-desethyl sunitinib (NDSUNI), regorafenib (REGO), nilotinib (NILO), dasatinib (DASA) and osimertinib (OSI) in human plasma/serum for therapeutic drug monitoring. The plasma/serum samples were deproteinated with acetonitrile after spiking with two deuterated internal standards (ISs, [ 2 H 8 ]-imatinib and [ 2 H 10 ]-sunitinib) and separated on a 40 °C ACQUITY UPLC® BEH C 18 column (1.7 µm, 2.1 mm × 50 mm). The mobile phase was composed of acetonitrile (solution A) and water-formic acid-ammonium acetate (1 M) (994:1:5, v/v/v, solution B). Gradient elution was applied at a flow rate of 0.4 mL/min. Detection was carried out using a Triple Quad 5500 tandem mass spectrometer coupled with an electrospray ionization (ESI) source in positive mode. The method was validated over the calibration curve (CV) range of 2–400 ng/mL for NDSUNI and DASA, 2.5–500 ng/mL for SUNI, 10–2000 ng/mL NDIMA and OSI, 20–4000 ng/mL for NILO, 30–6000 ng/mL for REGO and 50–10000 ng/mL for IMA using linear regression and 1/x 2 weighting. No difference was observed in the matrix effect (ME) among blank human plasma, hemolytic plasma, lipemic plasma, plasma spiked with ten commonly used drugs by cancer patients, or serum samples in general. The standard curve fitted by two standard curves of serum and plasma showed good linearity, and the precision and accuracy results of QC samples in both plasma and serum were acceptable and the concentration was comparable. To provide a clinical reference for the operation, the stability of the whole process from sample collection to drug detection was verified. SUNI and NDSUNI showed obvious photoisomerization under light exposure. Therefore, strict light protection was applied for all sample collection and handling steps of SUNI and NDSUNI. Compared with heparin anticoagulant tubes, the stability of the eight compounds in both whole blood and plasma was better in K3-EDTA and sodium citrate anticoagulant tubes. Given that all the analytes were stable in plasma at 4 °C for 48 h and in whole blood at room temperature for 48 h but OSI and REGO were unstable in whole blood and plasma at room temperature, samples should be centrifuged as soon as possible to be preserved as plasma at 4 °C when OSI or REGO is detected. In conclusion, this validated method can provide support for clinical practice, such as therapeutic drug monitoring (TDM) and pharmacokinetic studies of these six TKIs and two active metabolites.
研究领域:
药理学
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临床医学
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分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Food & Function
·
2021
·Vol. 12
·期 19
·8899-8906
·
IF 5.396
Qing Zheng,Yaru Hu,Ayuan Xiong,Ying Su,Zihao Wang,Kun Zhao,Yougui Yu
Elucidating the organometallic interactions in Baijiu will promote a deeper understanding of the flavour formation mechanism during Baijiu aging. However, the organometallic interactions during aging are difficult to explore because the concentration and status of metals in Baijiu samples are affected by other substances (such as organic acids), and the concentrations of these substances also change dynamically. Hence, the flavour formation mechanism of aged Baijiu was investigated based on a multi-method analysis (i.e. electrochemistry, ICP-MS/OES, and UPLC-Q-Orbitrap-MS/MS), which enabled us to solve the difficulty above. The key finding is that, in the aging period, the organic acids induce the transformation of the metal ion state from the complex state to the free state. As a result, the flavour compound (i.e. the esters) contents in aged Baijiu are regulated by the free metal ion-catalyzed reactions.
研究领域:
食品科学
·
分析化学
·
金属有机化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）