RSC Advances
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2026
·Vol. 16
·期 20
·18657-18665
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IF 6.1
Lu Li,Na Li,Wendan Niu,Aijing Guo,Ling Ma,Wei Zhao,Yawei Zhang,Ke Wang
β-Lactams (β-LAs) are a class of widely used antibiotics. However, their residues in food may pose a threat to human health. Therefore, it is of great necessity to develop a method that can sensitively and effectively detect β-LAs at trace levels in complex matrices. In this study, a novel functionalized magnetic covalent organic framework was synthesized based on biphenyl-3,3′,5,5′-tetracarbaldehyde and p-phenylenediamine. This material was used as an adsorbent for the effective extraction of 9 β-LAs in water and milk samples, which were analyzed by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The experimental parameters were optimized, then the sensitive and accurate detection method was developed with excellent linearity (R2 ≥ 0.9990), low limits of detection (0.001–0.347 µg L−1) and limits of quantitation (0.002–1.051 µg L−1) for β-LAs. Meanwhile, good recoveries (71.7–118.8%) of 9 β-LAs in water and milk samples were obtained with the relative standard deviations (RSD) <10% (n = 5). In conclusion, Fe3O4@SiO2@Ap-COF can be regarded as an effective magnetic adsorbent, and the established method holds significant promise for rapid detection of 9 β-LAs in water and milk samples.
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高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2025
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IF 3.1
Xiao-han Peng,Yan-lin Zhao,Zhong Huang,Xin-feng Xia,Kun Wang,Peng Jin,Yan Du,Dao-quan Tang
Currently, treatment with antiepileptic drugs (AEDs) is still the first choice for epileptic patients, while monitoring their blood concentrations is undoubtedly beneficial for minimizing their adverse side effects and optimizing their therapeutic effects. In this study, an ultra-high performance liquid chromatography coupled with tandem mass spectrometry with polarity switching was developed and validated for simultaneous determination of 14 AEDs and 2 active metabolites in human serum. Olanzapine was selected as the internal standard. One-step protein precipitation using methanol containing 0.05 % formic acid was used to treat sample, and the supernatant was injected for analysis without further evaporation and reconstitution. Chromatographic separation was performed on an Aglient Zorbax Eclipse Plus C18 (50 mm × 2.1 mm, 1.8 μm) column with gradient methanol and 0.1 % formic acid in water as mobile phase. Multi-reaction monitoring was performed for quantification of 16 analytes in polarity switching mode. Matrix-matched calibration curves of 16 analytes presented good linearity within the test concentration range ( r > 0.99). The intra- and inter-run accuracies and precisions at the lower limit of quantification, and low, medium and high quality control levels were all less than 20 % or 15 %, respectively. The extraction recovery, matrix effect, and stability were all acceptable under detected conditions. Finally, this method was successfully applied in the quantitation of target analytes in the serum of patients received AEDs.
研究领域:
药理学
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临床医学
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分析化学
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JOURNAL OF ETHNOPHARMACOLOGY
·
2024
·
IF 4.8
Tao Chen,Xian Zhou,Minxing Zhu,Xueting Chen,Dennis Chang,Yifan Lin,Wen Xu,Yanfang Zheng,Shaohua Li,Jianyuan Song,Mingqing Huang
Ethnopharmacological relevance Bronchitis is a respiratory disease characterized by a productive cough. Polygala tenuifolia Willd., commonly known as Yuan zhi , is a traditional Chinese herbal medicine used for relieving cough and removing phlegm. Despite its historical use, studies are lacking on the effectiveness of P. tenuifolia in treating bronchitis. Furthermore, the molecular mechanisms underlying the action of its bioactive compounds remain unknown. Aim of the study This study aims to identify the main bioactive compounds responsible for the effects of P. tenuifolia liquid extract (PLE) in treating bronchitis and to elucidate the associated molecular mechanisms. Materials and Methods The main chemical compounds in PLE were identified and determined using ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). The antitussive, expectorant and anti-inflammatory activities of PLE were evaluated in an ammonia-induced mouse cough model, a tracheal phenol red excretion mouse model, and a xylene-induced ear swelling mouse model, respectively. A network pharmacology analysis was conducted to investigate the associated gene targets, gene ontology, and KEGG pathways related to the main bio-actives in PLE targeting bronchitis. PLE and its five bioactive compounds were assessed for their potential anti-inflammatory activities in lipopolysaccharide (LPS)-stimulated RAW264.7 cells. Western blot analysis was conducted to elucidate the associated molecular mechanisms. Results Thirty-seven compounds in PLE were identified, and twelve main compounds were further quantified in PLE using UPLC-MS/MS. PLE oral gavage administrations (0.6 and 0.12 mg/kg) for 7 days markedly reduced cough frequency, prolonged latency period of cough, reduced phlegm and inflammation in mice. The network pharmacology analysis identified 57 gene targets of PLE against bronchitis. The PI3K/AKT and MAPK signalling pathways were the top two modulated pathways. In RAW264.7 cells, PLE (12.5-50 μg/mL) significantly reduced cyclooxygenase-2 (COX-2), inducible nitric oxide synthase (iNOS), interleukin (IL)-1β, IL-6 and tumor necrosis factor (TNF)-α. PLE downregulated LPS-elevated protein targets in both PI3K/AKT and MAPK signaling pathways. In PLE, tenuifolin, polygalaxanthone ⅠⅠⅠ, polygalasaponin ⅩⅩⅤⅢ, tenuifoliside B, and 3,6’-Disinapoyl sucrose, were identified as the top five core components responsible for treating bronchitis. These compounds were also found to modulate the protein targets in the PI3K/AKT and MAPK signalling pathways. Conclusions This study demonstrated the potential therapeutic effects of PLE on bronchitis by reducing cough, phlegm and inflammation. The anti-inflammatory action and molecular mechanisms of the 5 main bioactive compounds in PLE were partly validated through the in vitro assays. The findings provide valuable insights into the mechanisms underlying the traditional use of PLE for bronchitis.
研究领域:
药理学
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中药学
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分子生物学
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分析化学
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2021
·
IF 3.935
Maoyuan Jiang,Jiliang Cao,Chunbo Zhang,Biru Su,Shengpeng Wang,Na Ning,Ting Lei,Peng Li
Wushe Zhiyang Pills (WZP), a classical traditional Chinese medicine (TCM) formula, has been extensively used for the treatment of chronic urticaria and other relevant dermatologic diseases. In this study, a holistic method combining ultra-performance liquid chromatography coupled with diode array detector (UPLC-DAD) fingerprint and multi-components quantitative analysis was developed and validated for quality evaluation of WZP. As a result, a total of 34 characteristic peaks were screened to assess the chemical similarities of 16 batches of WZP samples. By coupling with a hybrid linear ion trap (LTQ)-Orbitrap mass spectrometer, 163 compounds were identified or tentatively identified in WZP. Furthermore, a rapid quantitative analysis method based on ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) technique was optimized and validated for simultaneously determination of 16 chemical markers within 13 min in WZP. The developed UPLC-MS/MS approach was successfully employed for analysis of 16 batches of WZP samples. The proposed comprehensive method combining holistic chemical profile with notable target compounds has proved to be suitable for the systematical quality evaluation of WZP, which provides a feasible and efficient strategy to monitor the overall quality consistency of TCM formulae.
研究领域:
中药学
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分析化学
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皮肤病学
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高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2016
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IF 3.169
Weiguo Liao,Jianye Yu,Zhonglin Guo,Wenqiang Ba,Ding Wang,Zhou Li,Wentao Fan,Fengyun Liao,Yinai Wu,Lisheng Wang
A rapid, sensitive and selective ultra-performance liquid chromatography tandem mass spectrometry (UPLC–MS/MS) method has been developed for the simultaneous determination and pharmacokinetic investigation of Tetramethylpyrazine (TMP) and Ferulic acid (FA) in rat striatum. The method was validated over the concentration range of 1.15–505 ng/mL for TMP and 3.23–101 ng/mL for FA, with a lower limit of quantitation (LLOQ) of 1.15 ng/mL and 3.23 ng/mL, respectively. This method can be successfully applied in pharmacokinetic studies of TMP and FA in striatum of awake and anesthetic rats. The cerebral blood flow velocity (CBF) during middle cerebral artery occlusion (MCAO) was monitored by Laser speckle contrast imaging, to observe whether the compatibility of TMP and FA could improve CBF against cerebral ischemia/reperfusion (I/R) injury. Infarct volume was examined to evaluate severity of ischemic brain injury. The pharmacokinetic study indicated that T 1/2, C max, MRT and AUC 0-inf were changed after combined administration of TMP and FA, when compared with either drug alone both in awake and anesthetic groups. The pharmacodynamics results showed that co-administration of drugs could enhance the CBF during middle cerebral artery occlusion and reduced the infarct volume. Taken together, the compatibility treatment of TMP and FA might be a promising therapeutic strategy for ischemic stroke. Further study is required to optimize the compatibility proportion.
研究领域:
药理学
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神经科学
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分析化学
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中风研究
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高影响因子
Food & Function
·
2019
·Vol. 10
·期 10
·6484-6491
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IF 3.241
Qiu Wu,Yan Zhao,Xiangnan Zhang,Xingbin Yang
Gut microbiota-dependent metabolites trimethylamine N-oxide (TMAO), trimethylamine (TMA) and dimethylamine (DMA) from dietary methylamines have recently gained much attention due to their high association with chronic kidney disease risk. Hence a simpler and faster performance liquid chromatography-tandem mass spectrometry method was developed and validated. The quantitative analysis was achieved within 6 min by using Agilent 6460C UPLC-MS/MS with 10% methyl alcohol isocratic elution and was more simple, convenient and rapid than that of previously reported methods. Furthermore, method verification results showed that the method correlation coefficient was 0.99978293, 0.99997514 and 0.98784721, and the detection limit was 0.121, 8.063 and 0.797 μg L−1, and the precision of the retention time and peak area of analytes was less than 0.331 and 3.280, respectively. The method was applied to simultaneously determine TMAO, TMA and DMA in the urine and serum from mice treated with normal, high L-carnitine, or high choline diet. Quantitative recoveries of TMAO, TMA and DMA were in the range of 94.2%–101.0%, and the RSD values were lower than 5.17%. The proposed UPLC-MS/MS-based assay should be of value for further evaluating TMAO as a risk marker and for examining the effect of dietary factors on TMAO metabolism.
研究领域:
分析化学
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生物化学
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代谢组学
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FOOD CHEMISTRY
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2026
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IF 10.4
Nan Deng,Hui Wang,Fangping Yin,Xiaobo Hu,Jijun Qin,Feifei Zhong,Ben Li,Wenting Cao,Peng Zhou
This study developed a rapid and sensitive ultra-performance liquid chromatography-tandem triple quadrupole mass spectrometry (UPLC-MS/MS) method to detect adulteration of high-value camellia oil and olive oil with lower-cost sesame, soybean, and peanut oils. Four characteristic markers-sesamin and sesamolin (sesame oil), 4′,7-dimethoxyisoflavone (soybean oil), and sativanone (peanut oil) were identified and quantified with high specificity. Method validation demonstrated excellent linearity ( r > 0.997), recoveries (70%–110%), and precision (RSD < 6.1%). The limits of detection were 0.025%–0.10% for sesame oil, 1.0%–5.0% for soybean oil and peanut oil. Adulteration model experiments and method comparison analysis confirmed reliable multi-component adulteration detection in complex matrices. Analysis of 106 commercial samples revealed adulteration rates of 16.0%(camellia oil) and 25.0%(olive oil), primarily with soybean oil. Notably, the analysis of two law enforcement samples confirmed adulteration with soybean oil, consistent with the official regulatory findings. This approach overcomes limitations of traditional methods, offering a robust tool for safeguarding oil authenticity and consumers' rights.
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2020
·
IF 3.209
Authors: Kan Wang,Ting Geng,Wei Jiang,Qiao Zhang,Yi Zhang,Pei-dong Chen,Ming-qiu Shan,Min Zhang,Yu-ping Tang,An-wei Ding,Li Zhang
Rubiae Radix et Rhizoma (called “Qiancao”, QC), the root and rhizome of Rubia cordifolia L., has been widely used in clinical practice for its excellent performance in removing blood stasis and haemostasis. However, after carbonization processing, significant changes occurred in chemical components of the charcoal of Rubiae Radix et Rhizoma (called “Qiancaotan”, QCT), which enhanced the performance in haemostasis and weakened the performance in removing blood stasis in clinic. In order to study the material basis of function variation during processing, a rapid, reliable, accurate and validated UPLC–MS/MS approach was established to determine twelve quinones in QC and QCT simultaneously. Meanwhile, the antithrombotic effect of target components on zebrafish thrombus model induced by phenylhydrazine (PHZ) was investigated. Chromatographic separation was accomplished on an ACQUITY UPLC C 18 column with acetonitrile–water containing 0.2 % (v/v) formic acid as mobile phase, at a flow rate of 0.30 mL/min. Quantitation was performed using multiple reaction monitoring (MRM) in positive and negative ion electrospray ionization (ESI). Furthermore, the activity evaluation studies showed that the reduction of removing blood stasis effect of QCT was due to the decrease of dehydro- α -lapachone, lapachol, rubioncolin C and mollugin. This study demonstrated that the method has been successfully applied to determine the content of twelve quinones responsible for the function variation of QCT, and provided a new insight into the material basis and the effect of eliminating stasis before and after processing of QC.
研究领域:
药理学
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分析化学
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中医药
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高影响因子
International Journal of Analytical Chemistry
·
2020
·
IF 1.678
Zhenzhen Ying,Jingyao Wei,Ruijuan Liu,Fang Zhao,Yifang Yu,Xin Tian
Osimertinib is a novel oral, potent, and irreversible epidermal growth factor receptor tyrosine kinase inhibitor (EGFR-TKI) for treatment of advanced T790M mutation-positive advanced non-small cell lung cancer, which is commonly combined with ginsenoside Rg3 in clinic to enhance the efficacy and minimize adverse reactions. In the present study, a highly sensitive UPLC-MS/MS method was established and validated for analysis of osimertinib in rat plasma according to US FDA guideline. Separation was performed on a C18 (2.1 × 50 mm, 2.6 μm) column using a gradient elution of ammonium formate (10 mM) with 0.1% formic acid buffer (A) and ACN (B) at a flow rate of 0.2 mL/min. Detection was carried out on a triple quadrupole tandem mass spectrometer equipped with electrospray ionization in the MRM mode. The method was validated over a concentration range of 1–400 ng/mL for osimertinib. The intra- and interday accuracy and precision values were within ±15%. No significant degradation occurred under the experimental conditions in stability assays. There was a further investigation on the effects of multiple doses of ginsenoside Rg3 on the pharmacokinetics of osimertinib in rats for the first time. The results implied that osimertinib exhibited a slow absorption and moderate-rate elimination in rats following oral administration. Coadministeration with ginsenoside Rg3 (5 mg/kg, 7 days, i.g.) may have no effect on the pharmacokinetics of osimertinib in rats. The results provide a reference for the clinical concomitant medications of Rg3 and osimertinib.
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高影响因子
BMC Pharmacology & Toxicology
·
2024
·Vol. 25
·期 1
·1-15
·
IF 2.8
Wang Tianyan,Tao Ting,Liu Yi,Dong Jie,Ni Shanhong,Liu Yun,Li Yanli,Xu Ning,Sun Zengxian
Background and purposes It is unclear whether the parent Saxagliptin (SAX) in vivo is the same as that in vitro, which is twice that of 5-hydroxy Saxagliptin (5-OH SAX). This study is to construct a Pharmacokinetic-Pharmacodynamic (PK-PD) link model to evaluate the genuine relationship between the concentration of parent SAX in vivo and the effect. Methods First, we established a reliable Ultra Performance Liquid Chromatography-Mass Spectrometry (UPLC-MS/MS) method and DPP-4 inhibition ratio determination method. Then, the T2DM rats were randomly divided into four groups, intravenous injection of 5-OH SAX (0.5 mg/kg) and saline group, intragastric administration of SAX (10 mg/kg) and Sodium carboxymethyl cellulose (CMC-Na) group. Plasma samples were collected at different time points for subsequent testing. Finally, we used the measured concentrations and inhibition ratios to construct a PK-PD link model for 5-OH SAX and parent SAX. Results A two-compartment with additive model showed the pharmacokinetic process of SAX and 5-OH SAX, the concentration-effect relationship was represented by a sigmoidal E max model and sigmoidal E max with E 0 model for SAX and 5-OH SAX, respectively. Fitting parameters showed SAX was rapidly absorbed after administration ( T max =0.11 h, t 1/2, ka =0.07 h), widely distributed in the body (V ≈ 20 L/kg), plasma exposure reached 3282.06 ng*h/mL, and the elimination half-life was 6.13 h. The maximum plasma dipeptidyl peptidase IV (DPP-4) inhibition ratio of parent SAX was 71.47%. According to the final fitting parameter EC 50 , EC 50, 5−OH SAX =0.46EC 50, SAX(parent) , it was believed that the inhibitory effect of 5-OH SAX was about half of the parent SAX, which is consistent with the literature. Conclusions The PK-PD link model of the parent SAX established in this study can predict its pharmacokinetic process in T2DM rats and the strength of the inhibitory effect of DPP-4 based on non-clinical data.
研究领域:
药理学
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药代动力学
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药效学
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糖尿病研究
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分析化学
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高影响因子
CURRENT PHARMACEUTICAL BIOTECHNOLOGY
·
2026
·Vol. 27
·期 1
·76-94
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IF 2.6
Zhixin Wang,Shuqin Liu,Ying Zhang,Huaming Xian,Xinzhu Yuan,Changwei Lin,Xisheng Xie
Background Diabetic Kidney Disease (DKD) is a major cause of End-Stage Renal Disease (ESRD) and lacks effective treatments. Tangmaikang Granules (TMK), a multi-herb traditional Chinese medicine formulation, have shown potential in managing DKD. However, the precise active components, molecular mechanisms, and therapeutic advantages of TMK remain unclear. Objective This study tests the hypothesis that TMK granules exert protective effects on DKD by targeting multiple pathways involved in oxidative stress, inflammation, and apoptosis in podocytes through a multi-targeted approach. The aim was to identify TMK’s bioactive components, evaluate its therapeutic potential, and uncover its molecular mechanisms in DKD. Methods The bioactive constituents in TMK were determined through ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Drug targets were identified using SwissTargetPrediction and SuperPred, whereas DKD-associated targets were obtained from the GeneCards, DisGeNET, OMIM, and TTD databases. A Protein-Protein Interaction (PPI) network was constructed, and key targets were identified via topological analysis. Molecular docking and dynamics simulations were performed to evaluate stable binding interactions. GO and KEGG pathway enrichment analyses were conducted to uncover relevant signaling pathways. TMK's effects on oxidative stress, inflammation, and apoptosis in podocytes were assessed using CCK-8, flow cytometry, RT-qPCR, ELISA, and Western blot assays. Results Thirty active compounds and 384 potential therapeutic targets were identified, with eight key targets. Pathway enrichment analysis revealed TMK’s involvement in AGE-RAGE, EGFR, HIF-1, and apoptosis pathways, affecting inflammatory cytokine responses and oxidative stress. In vitro experiments demonstrated that TMK significantly reduced oxidative stress, inflammation, and apoptosis in podocytes by inhibiting the MAPK and NF-κB pathways. Conclusion TMK granules target DKD through a multi-component, multi-target strategy, effectively mitigating oxidative stress and suppressing inflammatory and apoptotic pathways. This study integrates advanced computational and experimental methods, demonstrating TMK’s unique therapeutic potential and providing a robust foundation for its clinical application in DKD management.
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FOOD CHEMISTRY
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2026
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IF 10.4
Jialiang Zou,Huangsheng Zhang,Liang Zhao,Huanhuan Xu,Lin Chen,Hongping Chen,Fu Wang,Yuan Hu,Youping Liu
Chuan Chenpi (CCP), the peel of the ancient Chinese citrus variety Citrus reticulata ‘Dahongpao’, enhances its edible and medicinal value through aging. This study focuses on CCP samples aged 1–8 years, aiming to explore the dynamic changes during aging. Although aging induced noticeable changes in color, Fourier Transform Infrared (FTIR) analysis revealed no significant alterations in functional groups. Volatile and non-volatile metabolomic analyses indicated that aging primarily affects metabolite content rather than types, and both composition and antioxidant activity reached relatively high levels in the fourth year. The experimental results illustrate that the improvement in CCP quality induced by aging does not follow a linear pattern but exhibits fluctuations. The findings verify that the fourth year serves as a critical turning point for CCP's quality. This study clarifies the dynamic variation of chemical components in CCP during aging, thereby providing a scientific basis for the selection of its aging duration.
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高影响因子
危险品化学品经营许可证（带存储）