MOLECULES
·
2019
·Vol. 24
·期 16
·2906
·
IF 3.06
Da-Le Guo,Jin-Feng Chen,Lu Tan,Meng-Ying Jin,Feng Ju,Zhi-Xing Cao,Fang Deng,Li-Na Wang,Yu-Cheng Gu,Yun Deng
Two new terpene glycosides (1–2) along with two known analogs (3–4) were obtained from the root ofSanguisorba officinalis,which is a common traditional Chinese medicine (TCM). Their structures were elucidated by nuclear magnetic resonance (NMR), electrospray ionization high resolution mass spectrometry (HRESIMS), and a hydrolysis reaction, as well as comparison of these data with the literature data. Compounds1–4exhibited anti-inflammatory propertiesin vitroby attenuating the production of inflammatory mediators, such as nitric oxide (NO) as well as tumor necrosis factor-α (TNF-α) and interleukin-6 (IL-6). An anti-inflammatory assay based on the zebrafish experimental platform indicated that compound1had good anti-inflammatory activity in vivo by not only regulating the distribution, but also by reducing the amount of the macrophages of the zebrafish exposed to copper sulfate.Keywords:terpene glycosides;structural elucidation;Sanguisorba officinalis;zebrafish;anti-inflammatory
研究领域:
药理学
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化学
·
生物学
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PubMed
高影响因子
Food & Function
·
2019
·Vol. 10
·期 2
·824-835
·
IF 3.241
Xiaoxia Chen,Xin Hou,Degang Qing,Qian Zhang,Chunyan Yan
Humulus lupulus is distributed mainly in Asia, Europe, and North America, and the flowers and infructescences are used worldwide in beer brewing as an essential flavoring ingredient. In China, the main producing areas are the Xinjiang Uygur Autonomous Region and Gansu provinces. The annual production of H. lupulus in China accounts for about 13% of worldwide production, ranking third after the United States and Germany. The female flower of H. lupulus also is used in traditional Chinese medicine, but the bioactive components responsible for its benefits remain unclear. In this study, we isolated a homogeneous polysaccharide (HLP50-2) from female flowers of H. lupulus via DEAE-52 cellulose and Sephadex G-75 gel filtration chromatography. The molecular weight was 73.25 kDa. Chemical methods, gas chromatography-mass spectrometry, and nuclear magnetic resonance analyses showed that HLP50-2 consisted of →4)-β-D-GlcAp-(1→, →4)-α-L-Rhap-(1→, →5)-α-L-Araf-(1→, α-L-Araf-(1→, →3,6)-β-D-Galp-(1→, α-D-Galp-(1→, →3,4,6)-β-D-Galp-(1→, β-D-Xylp-(1→, →6)-α-D-Galp-(1→, and →4)-β-D-Galp-(1→. Advanced structural analysis indicated that HLP50-2 has a sheet-like structure with uneven distribution and the surface was smooth. In addition, we used MC3T3-E1 cells to evaluate the osteogenic activity of HLP50-2. The results show that HLP50-2 significantly promoted the proliferation, differentiation, and mineralization of MC3T3-E1 cells at concentrations of 12.5 μg mL−1 and 25 μg mL−1. In particular, at 25 μg mL−1, the promoting mineralization effect of HLP50-2 was better than that of the positive control, 17β-estradiol, and the alkaline phosphatase activity after 10 d of treatment was comparable to that of the positive control. The extraction, isolation, purification, structural identification, and osteogenic activity of H. lupulus polysaccharides suggest that homogeneous polysaccharide HLP50-2 has pronounced anti-osteoporosis activity. Therefore, it has broad application prospects in pharmaceutical industries and health-care products.
研究领域:
植物化学
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药理学
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生物医学
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PubMed
高影响因子
CHROMATOGRAPHIA
·
2022
·Vol. 86
·期 2
·185-197
·
IF 2.213
Lin Xinghua,Hao Gugu,Xu Guobin,Sun Fuzhou,Xin Libo,Wu Shuming,Wang Zhongqing,You Jinsong,Huang Fangfang,Song Xuezhi
An unknown peak with a relative retention time (RRT) of 1.47 was noticed in HPLC chromatograms for related substances of mirabegron extended-release tablets. The level of this unknown peak under the accelerated stability condition for 6 months was as high as 0.19%, which had a trend to exceed the identification threshold of 0.2% from ICH Q3B. The purpose of this study was to identify the RRT 1.47 impurity, and we studied its degradation mechanism to control its content to a lower level. The structure of the RRT 1.47 impurity was identified as a mirabegron dimer bridged by methylene via LC–MS and NMR. Investigation on compatibility of drug-excipients indicated that this impurity formed by Mannich reaction between mirabegron and residual formaldehyde in excipients polyethylene glycol (PEG), polyoxyethylene (PEO). Moreover, the determination of formaldehyde content in excipients further proved this speculation. There was a linear relationship between the amount of formaldehyde and the content of generated dimer impurity within a certain range. The reaction between mirabegron and formaldehyde at different temperatures demonstrated that the higher the temperature, the faster the reaction rate and the higher level of this impurity were generated. To understand the kinetics of the reaction, we calculated the rate of dimerization and also the activation energy of the process based on the stability data. During the development of pharmaceutical formulation on mirabegron or similar structure, appropriate excipients should be selected or the formaldehyde content in excipients could be controlled to avoid such reactions to improve the quality of the product.
研究领域:
药物化学
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制药工程
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DOI
高影响因子
ENVIRONMENTAL SCIENCE & TECHNOLOGY
·
2018
·
IF 6.653
Jing Chen,Nannan Wu,Xinxin Xu,Ruijuan Qu,Chenguang Li,Xiaoxue Pan,Zhongbo Wei,Zunyao Wang
Potassium ferrate [Fe(VI)] is a promising oxidant widely used in water treatment for the elimination of organic pollutants. In this work, the reaction kinetics, products, and mechanisms of the antimicrobial agent chlorophene (CP) undergoing Fe(VI) oxidation in aqueous solutions were investigated. CP is very readily degraded by Fe(VI), with the apparent second-order rate constant, k, being 423.2 M–1 s–1 at pH 8.0. A total of 22 oxidation products were identified using liquid chromatography–quadrupole time-of-flight–mass spectrometry , and their structures were further elucidated using tandem mass spectrometry. According to the extracted peak areas in mass spectra, the main reaction products were the coupling products (dimers, trimers, and tetramers) that formed via single-electron coupling. Theoretical calculations demonstrated that hydrogen abstraction should easily occur at the hydroxyl group to produce reactive CP· radicals for subsequent polymerization. Cleavage of the C–C bridge bond, electrophilic substitution, hydroxylation, ring opening, and decarboxylation were also observed during the Fe(VI) oxidation process. In addition, the degradation of CP by Fe(VI) was also effective in real waters, which provides a basis for potential applications.
研究领域:
环境科学
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化学
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PubMed
高影响因子
Scientific Reports
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2021
·Vol. 11
·期 1
·1-8
·
IF 4.38
Xu Xue,Naseri Ali,Houbraken Jos,Akbari Farzaneh,Wang Xiaodong,Zhao Rongfen,Zhang Hong,Najafzadeh Mohammad Javad,Deng Shuwen
Aspergillus species are emerging causative agents of non-dermatophyte mold onychomycosis. In this study, 48 Aspergillus isolates were obtained from patients with onychomycosis in Mashhad, Iran, during 2015–2018. The aim is to identify the Aspergillus isolates to the species level by using partial calmodulin and beta-tubulin gene sequencing and MALDI-TOF MS, and to evaluate their in vitro susceptibility to ten antifungal drugs: terbinafine, itraconazole, voriconazole, posaconazole, ravuconazole, isavuconazole, caspofungin, micafungin, anidulafungin and amphotericin B according to CLSI M38-A3. Our results indicate that A.flavus (n = 38, 79%) is the most common Aspergillus species causing onychomycosis in Mashhad, Iran. Other detected species were A. terreus (n = 3), A. tubingensis (n = 2), A. niger (n = 1), A. welwitschiae (n = 1), A. minisclerotigenes (n = 1), A. citrinoterreus (n = 1) and A. ochraceus (n = 1). Aspergillus flavus , A. terreus and A. niger isolates were correctly identified at the species level by MALDI-TOF MS, while all cryptic species were misidentified. In conclusion, A. flavus is the predominant Aspergillus species causing onychomycosis due to Aspergillus spp. in Mashhad, Iran. MALDI-TOF MS holds promise as a fast and accurate identification tool, particularly for common Aspergillus species. It is important that the current database of reference spectra, representing different Aspergillus species is expanded to increase the precision of the species-level identification. Terbinafine, posaconazole and echinocandins were i n vitro most active against the studies Aspergillus isolates and terbinafine could be the first choice for treatment of onychomycosis due to Aspergillus .
研究领域:
医学
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真菌学
·
临床微生物学
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PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2021
·
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
·
药学
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DOI
PubMed
高影响因子
Journal of Forensic and Legal Medicine
·
2024
·
IF 1.2
Zhonghao Yu,Yuhao Yuan,Qing Shi,Hang Gao,Erjuan Zhao,Jinghong Ma,Yiwu Zhou
Brodifacoum, a long-acting anticoagulant rodenticide, exerts inhibitory effects on blood coagulation factor synthesis, leading to abnormal clotting function and potential fatality. Poisoning of accidental exposure to brodifacoum is not rare, but death from brodifacoum poisoning can be largely avoided with timely and long-term effective treatments, consequently, forensic data on fatalities due to brodifacoum poisoning may be limited. This paper presents a case of brodifacoum-induced homicide, detailing the medial records and pathological changes observed in multiple organs. Furthermore, t liquid chromatography–tandem mass spectrometry (LC-MS/MS) was employed to measure the concentrations of brodifacoum in blood, hydropericardium, and urine 40 days post-poisoning (1 day post-mortem), yielding values of 0.097 μg/mL, 0.089 μg/mL, and 0.007 μg/mL respectively. The aim of this article is to contribute towards forensic identification of fatalities resulting from brodifacoum poisoning while also serving as a reference for clinical diagnosis in similar cases.
研究领域:
法医学
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毒理学
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DOI
PubMed
高影响因子
Journal of Functional Foods
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2017
·
IF 3.144
Shan Hong,Shanshan Wu,He Cai,Yimin Wang,Songbai Liu
Proton NMR signals of the phenolic hydroxyl groups of the substituted catechins were successfully collected. The identities of these signals were elucidated and confirmed by a combination of computational and experimental investigations including GIAO-B3LYP NMR chemical shift calculation, kinetic analysis of acylation, and NOESY correlation. Furthermore, the reliability of chemical shifts of hydrogens of phenolic hydroxyl groups was confirmed by evaluation of the influence of acidic, basic and water residues. Finally, the chemical shift profiles of phenolic hydroxyl groups were developed for instant structural recognition. This study demonstrated the feasibility of application of chemical shifts of hydrogens of phenolic hydroxyl groups as fingerprint for structural determination and the concept could be extended to other polyphenols.
研究领域:
植物化学
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分析化学
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计算化学
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DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2018
·
IF 3.716
Guozhu Liu,Baolei Luan,Guiting Liang,Libo Xing,Liang Huang,Changyun Wang,Ying Xu
Capreomycin has good clinical utility to treat multidrug resistant tuberculosis, but it is only used as a second line drug due to its adverse reactions. Literature has demonstrated that the toxicity of capreomycin product is significantly influenced by the impurities in it. Unfortunately, so far, no one impurity in capreomycin has ever been isolated and definitely identified due to its extremely strong basic character and high polarity. An ion-pair method reported in literature can provide separation of capreomycin and its impurities, but it is hard to be used for the preparative purpose. In this study, this ion-pair method was further improved to detect more impurities in capreomycin sulfate substance. Besides the four main components (IA, IB, IIA and IIB), four impurities (impurity A–D) with their contents much higher than the identification threshold were observed. Furthermore, a two dimensional (2D) LC quadrupole-time of flight (Q-TOF) MS method was established to realize high resolution MS analysis of these impurities. For the purpose of preparative isolation, a hydrophilic interaction chromatography (HILIC) method was established. The four main components were well isolated, but unfortunately, the four impurities were co-eluted with each other or with IB by the HILIC method. Fortunately, the degradation experiments revealed that IA and IB could yield clean impurity A and B respectively in acidic medium, and can yield clean impurity D and C respectively in alkaline medium. Therefore, IA and IB were first isolated by the preparative HILIC method, then pure IA and IB underwent acid degradation and base degradation separately and followed by re-isolation by the HILIC method to obtain pure impurity A–D respectively. Based on Q-TOF MS and NMR analysis, the structures (including absolute configuration) of the four isolated impurities were definitely identified.
研究领域:
药物化学
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分析化学
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PubMed
高影响因子
Foods
·
2021
·Vol. 10
·期 11
·2888
·
IF 4.35
Shuang Chen,Jialing Lu,Michael Qian,Hongkui He,Anjun Li,Jun Zhang,Xiaomei Shen,Jiangjing Gao,Yan Xu
This paper proposes the combination of headspace-gas chromatography-ion mobility spectrometry (HS-GC-IMS) and chemometrics as a method to detect the age of Chinese liquor (Baijiu). Headspace conditions were optimized through single-factor optimization experiments. The optimal sample preparation involved diluting Baijiu with saturated brine to 15% alcohol by volume. The sample was equilibrated at 70 °C for 30 min, and then analyzed with 200 μL of headspace gas. A total of 39 Baijiu samples from different vintages (1998–2019) were collected directly from pottery jars and analyzed using HS-GC-IMS. Partial least squares regression (PLSR) analysis was used to establish two discriminant models based on the 212 signal peaks and the 93 identified compounds. Although both models were valid, the model based on the 93 identified compounds discriminated the ages of the samples more accurately according to the goodness of fit value (R2) and the root mean square error of prediction (RMSEP), which were 0.9986 and 0.244, respectively. Nineteen compounds with variable importance for prediction (VIP) scores > 1, including 11 esters, 4 alcohols, and 4 aldehydes, played vital roles in the model established by the 93 identified compounds. Overall, we determined that HS-GC-IMS combined with PLSR could serve as a rapid and accurate method for detecting the age of Baijiu.Keywords:Chinese liquor (Baijiu);ageing discrimination;HS-GC-IMS;extraction condition optimization
研究领域:
分析化学
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食品科学
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DOI
PubMed
高影响因子
MOLECULES
·
2020
·Vol. 25
·期 5
·1082
·
IF 3.267
Limin Li,Bin Hao,Yulong Zhang,Shen Ji,Guixin Chou
Militarine, a natural glucosyloxybenzyl 2-isobutylmalate, isolated fromBletilla striata, was reported with a prominent neuroprotective effect recently. The limited information on the metabolism of militarine impedes comprehension of its biological actions and pharmacology. This study aimed to investigate the metabolite profile and the distribution of militarine in vivo, which help to clarify the action mechanism further. A total of 71 metabolites (57 new metabolites) in rats were identified with a systematic method by ultra-high-performance liquid chromatography combined with quadrupole time-of-flight tandem mass spectrometry (UPLC-Q-TOF-MS/MS). The proposed metabolic pathways of militarine include hydrolyzation, oxidation, glycosylation, esterification, sulfation, glucuronidation and glycine conjugation. Militarine and its metabolites were distributed extensively in the treated rats. Notably, six metabolites of militarine were identified in cerebrospinal fluid (CSF), which were highly consistent with the metabolites after oral administration of gastrodin in rats. Among the metabolites in CSF, five of them were not reported before. It is the first systematic metabolic study of militarine in vivo, which is very helpful for better comprehension of the functions and the central nervous system (CNS) bioactivities of militarine. The findings will also provide an essential reference for the metabolism of other glucosylated benzyl esters of succinic, malic, tartaric and citric acids.Keywords:militarine;metabolite identification;metabolic profiles;UPLC-Q-TOF-MS/MS
研究领域:
药理学
·
分析化学
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产品关联
DOI
PubMed
高影响因子
Jove-Journal of Visualized Experiments
·
2022
·
IF 1.424
Wei Zhu,Weihua Chu
Hydrogen sulfide (H2S) is a toxic gas produced by bacteria in the proteolysis of sulfur-containing amino acids and proteins that plays an important role in human health. The H2S production test is one of the important bacterial biochemical identification tests. The traditional methods are not only tedious and time-consuming but also prone to inhibition of bacterial growth due to the toxic effect of heavy metal salts in sulfur-containing medium, which often leads to negative results. Here, we established a simple and sensitive method to detect H2S in bacteria. This method is a modified version of bismuth sulfide (BS) precipitation that uses 96-well transparent microtiter plates. Bacterial culture was combined with bismuth solution containing L-cysteine and cultivated for 20 min, at the end of which a black precipitate was observed.The visual detection limit for H2S was 0.2 mM. Based on the visual color change, the simple, high-throughput, and rapid detection of H2S producing bacteria can be achieved. In summary, this method can be used to identify H2S production in bacteria.
研究领域:
微生物学
·
医学检验
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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）