JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2021
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IF 3.935
Xing Han,Fang-jie Cheng,Bin Di,Hui Xu,Min Song,Tai-jun Hang,Yu-Ting Lu
Zopiclone, a non-benzodiazepine hypnotic, is the first-line treatment for insomnia. The quality and stability of zopiclone tablets directly affects its efficacy and safety. However, the impurity investigation in zopiclone tablets remain incomplete. In this study, the accelerated and long-term stabilities of zopiclone tablets, as well as the stability characteristics under thermal and photolytic conditions were evaluated according to the ICH guidelines. In addition, a sensitive and specific LC-QTOF-MS method was developed for the separation and identification of all the impurities in zopiclone tablets and its stability test samples. Nine impurities were found in the test samples, five among them have not been reported before. Based on the accurate mass and elemental compositions of the parent and product ions obtained, the structures of all the detected impurities were identified. Combined with the formulation composition analysis and stability studies, the origins and the formation mechanisms of these impurities were elucidated. The obtained results are useful for the establishment of the optimum formulation, storage condition, manufacturing processes and quality control of zopiclone tablets.
研究领域:
药物化学
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分析化学
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药学
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PubMed
高影响因子
Chemistry Africa-A Journal of the Tunisian Chemical Society
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2023
·Vol. 6
·期 4
·1799-1810
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IF 2.6
Gogoi Pinku,Kumar Amit,Das Aparoop,Baishya Gakul
The present study was aimed to investigate the role of Dillenia indica L. bark extracts and their kinetics of inhibition against the tyrosinase enzyme. The kinetics study of various concentrations of the extracts was executed by spectrophotometric assay. Out of four extracts, only hydro-ethanolic extract of D. indica barks (HEEBDI) showed the maximum radical scavenging capacity (36.73 ± 1.65 μg/ml) compared to ascorbic acid. Additionally, HEEBDI scavenging capacity and tyrosinase inhibitory properties showed a significant correlation. In HEEBDI, fifteen marker compounds were identified by LC-QTOF-MS method. The tyrosinase inhibitory activity of HEEBDI (IC 50 19.32 ± 0.57 μg/ml) showed a significant value compared to kojic acid (IC 50 22.08 ± 0.19 μg/ml). The inhibitory mechanism was confirmed in a mixed manner by enzyme kinetics. With minimal conformational energy, betulinic acid and kaempferol bind to the tyrosinase enzyme (PDB ID: 2y9x) as proved by their respective docking score and binding interaction.
研究领域:
植物化学
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药理学
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生物信息学
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高影响因子
Foods
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2021
·Vol. 10
·期 11
·2709
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IF 4.35
Yan Huang,Dandan Pu,Zhilin Hao,Xiao Yang,Yuyu Zhang
This work aims to explore the contribution of prickly ash (Zanthoxylum bungeanumMaxim) on the taste perception of stewed sheep tail fat. Liquid chromatography-tandem quadrupole time of flight mass spectrometry (LC-QTOF-MS) was applied to analyze the taste-related compounds. A total of 99 compounds in different sheep tail fat samples were identified. The semi-quantitative results showed that there were differences between the samples. The partial least squares discriminant analysis (PLS-DA) model without overfitting was used to investigate the effect of prickly ash. Eleven marker compounds were predicted with a variable importance for projection > 1, fold change > 2 andp< 0.05. An additional experiment showed that guanosine 5′-monophosphate, malic acid, inosine and adenosine 5′-monophosphate could improve the umami and saltiness taste of stewed sheep tail fat.Keywords:sheep tail fat;taste compounds;LC-QTOF-MS;PLS-DA;sensory analysis;additional experiment
研究领域:
食品科学
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化学计量学
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植物学
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PubMed
高影响因子
Journal of Pharmaceutical Analysis
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2024
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IF 6.1
Chengyi Zuo,Jingwei Zhou,Sumin Bian,Qing Zhang,Yutian Lei,Yuan Shen,Zhiwei Chen,Peijun Ye,Leying Shi,Mao Mu,Jia-Huan Qu,Zhengjin Jiang,Qiqin Wang
Dynamic tracking analysis of monoclonal antibodies (mAbs) biotransformation in vivo is crucial, as certain modifications could inactivate the protein and reduce drug efficacy. However, a particular challenge (i.e. immune recognition deficiencies) in biotransformation studies may arise when modifications occur at the paratope recognized by the antigen. To address this limitation, a multi-epitope affinity technology utilizing the MOF@Au@peptide@aptamer composite material was proposed and developed by simultaneously immobilizing complementarity determining region (CDR) mimotope peptide (HH24) and non-CDR mimotope aptamer (CH1S-6T) onto the surface of MOF@Au nanocomposite. Comparative studies demonstrated that MOF@Au@peptide@aptamer exhibited significantly enhanced enrichment capabilities for trastuzumab variants in comparison to mono-epitope affinity technology. Moreover, the higher deamidation ratio for LC-Asn-30 and isomerization ratio for HC-Asn-55 can only be monitored by the novel bioanalytical platform based on MOF@Au@peptide@aptamer and LC-QTOF-MS. Therefore, multi-epitope affinity technology could effectively overcome the biases of traditional affinity materials for key sites modification analysis of mAb. Particularly, the novel bioanalytical platform can be successfully used for the tracking analysis of trastuzumab modifications in different biological fluids. Compared to the spiked PB model, faster modification trends were monitored in the spiked serum and patients’ sera due to the catalytic effect of plasma proteins and relevant proteases. Differences in peptide modification levels of trastuzumab in patients’ sera were also monitored. In summary, the novel bioanalytical platform based on the multi-epitope affinity technology holds great potentials for in vivo biotransformation analysis of mAb, contributing to improved understanding and paving the way for future research and clinical applications.
研究领域:
药学
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分析化学
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生物技术
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生物化学
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PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2018
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IF 2.831
Yuting Lu,Xiyang Sun,Fan Song,Lei Wang,Min Song,Taijun Hang
An LC-QTOF-MS method was developed for the separation and characterization of related substances in varenicline tartrate. The separation was established on an InertSustain C18 column (4.6 mm × 150 mm, 5 μm) by liner gradient elution using 0.05% trifluoroacetic acid as mobile phase A and acetonitrile as mobile phase B. The degradation studies were conducted under the ICH prescribed stress conditions. Varenicline tartrate was found to be unstable to alkaline, oxidative, thermal and photolytic stresses, while relatively stable under acid stress condition. Thirteen related substances were detected all together in varenicline tartrate and its stressed samples. Their structures were identified mainly through positive ESI high resolution QTOF mass spectrometric analysis of the parent and product ions' accurate masses and the calculated elemental compositions. Among the 13 related substances, seven were process-related and six were degradation products, and two of them were further verified by chemical synthesis and NMR spectroscopic determination. Their formation mechanisms were also discussed, and the key steps in the manufacturing processes were also determined to provide varenicline tartrate with high purity.
研究领域:
药物化学
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分析化学
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制药工程
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DOI
PubMed
高影响因子
FOOD CHEMISTRY
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2022
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IF 9.231
Na Yan,Xia Li,Chundi Zhou,Qin Jiang,Jiyu Li,Zhenqing Zhang,Yilan Ouyang,Duxin Li,Jianxiang Li
Carrageenan (CGN) belongs to the sulfated polysaccharides family that is commonly used in the food industry. For oligosaccharide analysis, a liquid chromatography quadrupole time-of-flight/mass spectrometry strategy was developed using a hypothetical database. There are 2100 structures in the developed hypothetical κ-CGN database. To eliminate false-positive results, three approaches were used, including size exclusion chromatography with mass spectrometry, which differentiates the loss of sulfated groups caused by the hydrolysis process or the ionization process. Profiling of acidic hydrolysis products of κ-CGN was found that after 12 h of HCl cultivation, the κ-CGN was hydrolyzed to oligosaccharides lower than the degree of polymerization 10, breaking the α-1,3-glycoside linkage and producing even-numbered oligosaccharides. Another finding was that the pH at which acidic hydrolysis is terminated affects the generation of even and odd oligosaccharides. Peeling reaction occurs at the reduction end 4-linked-3,6-anhydrous- d -galactose when adjusted to alkaline conditions, thus generating odd oligosaccharides.
研究领域:
食品科学
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分析化学
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质谱分析
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DOI
PubMed
高影响因子
MOLECULES
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2023
·Vol. 28
·期 2
·656
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IF 4.6
Chanyi Li,Jiaying Qin,Wuping Liu,Bo Lv,Ning Yi,Jinfeng Xue,Zhigang Xue
Background: Homocysteine (Hcy) has been found to be closely related to the occurrence of diabetes mellitus (DM) and is considered as one of the risk factors of DM. However, Hcy alone is not enough as a factor to predict DM, and our study analyzed and determined the relationship between the main metabolites involved in the Hcy metabolic pathway and DM. Methods: A total of 48 clinical samples were collected, including 18 health control samples and 30 DM samples. All standards and samples were detected by LC-QTOF-MS. Multivariate statistical analysis and k-means cluster analysis were performed to screen and confirm the metabolites significantly correlated with DM. Results: A total of 13 metabolites of the Hcy metabolic pathway were detected in the samples. The content of Hcy, cysteine, taurine, pyridoxamine, methionine, and choline were significantly increased in the DM group (p< 0.05). Hcy, choline, cystathionine, methionine, and taurine contributed significantly to the probabilistic principal component analysis (PPCA) model. The odds ratios (OR) of Hcy, cysteine, taurine, methionine, and choline were all greater than one. K-means cluster analysis showed that the Hcy, taurine, methionine, and choline were significantly correlated with the distribution of glucose values (divided into four levels: 10.5–11.7 mmol/L, 7.7–9.7 mmol/L, 6.0–6.9 mmol/L, and 5.0–5.9 mmol/L, respectively). Conclusion: Hcy, taurine, methionine, and choline can be used as risk factors for diabetes diagnosis and are expected to be used for the assessment of diabetes severity.Keywords:homocysteine metabolism;diabetes;LC-MS;clinical diagnosis
研究领域:
代谢组学
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糖尿病研究
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临床化学
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PubMed
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Food Analytical Methods
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2026
·Vol. 19
·期 2
·91
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IF 3
Sun Weichao,Liu Huahong,Wu Yuxin,Qin Yuqi,Zhang Yu,Jin Wenying,Hai Hong,Zhang Yun,Nie Jinfang,Fu Haiyan
The geographical provenance of agricultural products is a key determinant of quality and economic value. An untargeted metabolomics-based ML pipeline was established to authenticate the origin of Yongfu Luohan Guo. LC-QTOF/MS profiling of samples from multiple origins generated comprehensive metabolite datasets, which were analyzed using supervised ML algorithms. Multivariate analysis revealed distinct metabolic signatures differentiating Yongfu and non-Yongfu Luohan Guo. The CNN algorithm outperformed other models, achieving 100% classification accuracy using 8 key metabolites These biomarkers include two flavonoids: 5-hydroxy-3-(5-hydroxy-2,4-dimethoxyphenyl)-6-methoxy-7-[3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxychromen-4-one and glabrol; three terpenoids: rhodojaponin III, lapidin, and acetylcimigenol arabinoside; and three alkaloids: corynoxeine, indirubin, and hydroquinidine. Region-specific metabolite accumulation trends were observed in Yongfu Luohan Guo, correlating with fruit quality attributes. This metabolomics-ML integration strategy presents a scalable solution for geographical indication authentication of diverse agricultural products. Graphical
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Natural Product Communications
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2024
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IF 1.5
Hui-Peng Song,Ming-Yue Zhao,Zhi-Li Xu,Jia-Nuo Zhang,Wen-Yu Wang,Zi-Xuan Ding,Ying Wang,Li-Bin Zhan,Xi Chen,Ruo-Nan Li,Yue-Hua Chen
ObjectivesThe aim is to discover α-glucosidase/acetylcholinesterase inhibitors as lead compounds from a traditional herbal prescription of Qi-Li-Qiang-Xin capsule (QLQX).MethodsA novel strategy combining time-based fractionation, LC-QTOF-MS, enzymatic activity assay, molecular docking and component-target association analysis was performed to discover α-glucosidase/acetylcholinesterase inhibitors from QLQX. Time-based fractionation combined with enzymatic activity assay was used to find the distribution period of active compounds in the herbal prescription. LC-QTOF-MS was used to analyze the structure of active compounds. Molecular docking was applied to explore the interaction between active compounds and targets.ResultsAccording to time-based fractionation, the active components of QLQX for acetylcholinesterase were primarily concentrated in the highly polar region, whereas the active components for α-glucosidase were predominantly found in the moderately polar area. A total of 33 compounds were identified by comparing with chemical reference substances. Dihydrotanshinone Ⅰ (16.98 µM), hydroxysafflor yellow A (84.57 µM), salvianolic acid A (76.62 µM) and cryptotanshinone (112.68 µM) were identified as acetylcholinesterase inhibitors from QLQX. Similarly, rosmarinic acid (62.29 µM), isochlorogenic acid A (17.95 µM), 4,5-dicaffeoylquinic acid (117.93 µM), danshensu (207.88 µM), salvianolic acid A (1.31 µM), 3,4-dicaffeoylquinic acid (91.71 µM), formononetin (67.26 µM), ginsenoside Rd (3.43 µM), ginsenoside Rb1 (26.37 µM) and ginsenoside F1 (18.79 µM) were discovered as α-glucosidase inhibitors. Notably, salvianolic acid A inhibited both acetylcholinesterase and α-glucosidase. The results of molecular docking indicated that hydrogen bonds, hydrophobic interactions and Pi-Pi T-shaped interactions were crucial for inhibiting acetylcholinesterase. Meanwhile, hydrogen bonds, hydrophobic interactions and Pi-Pi stacked interactions were significant in suppressing α-glucosidase.ConclusionQLQX contains numerous acetylcholinesterase and α-glucosidase inhibitors, demonstrating its potential therapeutic benefits for Alzheimer's disease and diabetes.
研究领域:
药理学
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中药学
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药物发现
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生物化学
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分子生物学
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产品关联
DOI
高影响因子
危险品化学品经营许可证（带存储）