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Four copper(II)-plumbagin and -bipyridine complexes (Cu1-Cu4) were synthesized as chemodynamic therapy agents with enhanced antitumor activity. As lipophilic and positively charged compounds, Cu1-Cu4 were preferentially accumulated in mitochondria and activated the mitochondrial apoptosis pathway. Mechanistic studies showed that Cu1-Cu4 reacted with GSH to reduce Cu2+ ions to Cu+ ions, catalyzed the formation of toxic hydroxyl radicals (ËOH) from hydrogen peroxide (H2O2) through a Fenton-like reaction, induced mitochondrial dysfunction, and activated caspase-9/3, which eventually led to apoptosis. Cu1-Cu4 arrested HeLa cells in the S phase and eventually killed cancer cells. Cu2 showed a favorable pharmacokinetic profile in mice. Moreover, Cu2 effectively inhibited the growth of HeLa xenografts in nude mice and showed low toxicity in vivo.
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Cobre , Naftoquinonas , Neoplasias , Humanos , Animais , Camundongos , Cobre/metabolismo , Peróxido de Hidrogênio/metabolismo , Células HeLa , Camundongos Nus , Mitocôndrias/metabolismo , Linhagem Celular Tumoral , Neoplasias/metabolismo , Glutationa/metabolismoRESUMO
To reveal the utilization value of leaf, stem, and root of Artemisia argyi, a rapid online liquid microextraction combined with a high-performance liquid chromatography coupled with 2,2-nitrogen-di (3-ethyl-benzothiazole-6-sulfonic acid) diammonium salt antioxidant assay system was established for analysis of antioxidants in the leaf, stem, and root of A. argyi, and a calibration quantitative method of antioxidant activity with equivalent chlorogenic acid was proposed. Thirty-three positive peaks were identified; among them, 12 compounds were found that possess good antioxidant activity including eleven organic acids (components 2-4, 8, 11-14, 17, 19, and 21) and one flavonoids (component 22). The proposed calibration quantitative method avoided the influence of content of compound and compared the extent of radical scavenging capacity of five antioxidant compounds, which were ranked as follow: 3,5-dicaffeoylquinic acid > 3,4-dicaffeoylquinic acid ≈ 4,5-dicaffeoylquinic acid > 1,4-dicaffeoylquinic acid > chlorogenic acid. In conclusion, this study provided composition and biological potential for the future development of the leaf, stem, and root of A. argyi. It is believed that the online liquid microextraction combined with high-performance liquid chromatography based antioxidant assay system can be widely used for the rapid screening of natural antioxidant components in the different parts of natural products.
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Artemisia , Medicamentos de Ervas Chinesas , Cromatografia Líquida de Alta Pressão/métodos , Antioxidantes/análise , Medicamentos de Ervas Chinesas/análise , Artemisia/química , Ácido Clorogênico/análise , Calibragem , Folhas de Planta/químicaRESUMO
Fangwen Jiuwei Decoction is a traditional Chinese medicine preparation for the treatment of pneumonia developed by Shenzhen Bao'an Chinese Medicine Hospital, which shows remarkable clinical responses. Qualitative and quantitative analyses of the main active compounds are crucial for the quality control of traditional Chinese medicine prescription in clinical application. In this study, we identified nine active compounds essential for the pharmacological effects of Fangwen Jiuwei Decoction based on the analysis of the Network Pharmacology and relevant literature. Moreover, these compounds can interact with several crucial drug targets in pneumonia based on molecular docking. We applied high-performance liquid chromatography-tandem mass spectrometry method was established these nine active ingredients' qualitative and quantitative detections. The possible cleavage pathways of nine active components were determined based on secondary ions mass spectrometry. The results of high-performance liquid chromatography-tandem mass spectrometry were further validated, which show a satisfactory correlation coefficient (r > 0.99), recovery rate (≥93.31%), repeatability rate (≤5.62%), stability (≤7.95%), intra-day precision (≤6.68%), and inter-day precision (≤9.78%). The limit of detection was as low as 0.01 ng/ml. In this study, we established a high-performance liquid chromatography-tandem mass spectrometry method to qualitatively and quantitatively analyze the chemical components in the Fangwen Jiuwei Decoction extract.
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Medicamentos de Ervas Chinesas , Medicamentos de Ervas Chinesas/análise , Espectrometria de Massas em Tandem/métodos , Simulação de Acoplamento Molecular , Medicina Tradicional Chinesa , Cromatografia Líquida de Alta Pressão/métodosRESUMO
Mahuang Xuanfei Zhike (MXZ) syrup, a Chinese patent medicine, has been widely used in the clinical treatment of cough. However, there is no reported method for the quantitative analysis of the effective components of MXZ syrup in biological samples. In this study, the effective components of MXZ syrup were screened by network pharmacology and molecular docking technology. A sensitive and rapid ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was established to test the active components of MXZ syrup in rat plasma and tissue homogenates, including ephedrine, amygdalin, chlorogenic acid, harpagoside, forsythin and forsythoside A. Chromatographic separation was performed on a Waters Acquity UPLC HSS T3 column (2.1 × 50 mm, 1.8 µm) and the mass analysis was conducted using a Waters Xevo TQ mass spectrometer using multiple reaction positive and negative ion simultaneous monitoring mode. The results showed that the linearity ranged from 0.3 to 409.4 ng/ml. The extraction recoveries were all <8.33%, and the matrix effects were all <8.45, which met the requirements. The pharmacokinetic and tissue distribution results indicated that the main active components of MXZ syrup were absorbed quickly and eliminated slowly in vivo, and there may be a reabsorption process.
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Medicamentos de Ervas Chinesas , Ephedra sinica , Ratos , Animais , Cromatografia Líquida , Espectrometria de Massas em Tandem/métodos , Cromatografia Líquida de Alta Pressão/métodos , Distribuição Tecidual , Simulação de Acoplamento Molecular , Medicamentos de Ervas Chinesas/farmacocinéticaRESUMO
BACKGROUND: The outbreak has had a devastating impact, and efforts are underway to speed up vaccination. The study's objective was to describe the clinical characteristics of the coronavirus disease 2019 (COVID-19) vaccination clinic in the Second People's Hospital of Fujian Province, China. Meanwhile, we monitored all the vaccine recipients to evaluate adverse reactions. METHODS: A cross-sectional study was done at the COVID-19 Vaccination Clinic, the Second People's Hospital of Fujian Province, China. We systematically collected Clinical data from the COVID-19 vaccination clinic between March 11 and November 11, 2021, including the type of vaccine, number of doses, gender, age, educational level, occupational category, adverse reactions, etc. Investigators will contact vaccine recipients by means of phone call or WeChat message to record the negative responses. Last, this report covers data through 8 mo, so it will be better to Evaluate the Safety of 2 inactivated COVID-19 vaccines from China (BBIBP-CorV [Beijing Institute of Biological Products, Beijing, China] and CoronaVac [Sinovac Life Sciences, Beijing, China]). RESULTS: The results indicated that the Second People's Hospital of Fujian Province received a total of 64,602 COVID-19 vaccines from March 11 to November 11, 2021, including 34,331 (53.14%) first doses, 29,245 (45.27%) second doses, and 1026 (1.59%) third doses. This study found the highest proportion in other personnel (38.69% at the first dose, 38.75% at the second dose, and 2.44% at the third dose), who were mainly retirees. People with higher levels of education are more likely to be vaccinated against COVID-19 during the early stages of vaccine rollout. In terms of age stratification, the highest proportion was found among people aged 18-49 (BBIBP-CorV: first dose 61%, second dose 62.6%, and third dose 76.8%; CoronaVac: first dose 66.1%, double dose 63.6%, and third dose 75.5%), followed by those over 60. The common adverse reactions were mainly local and systemic, and there were some differences between the 2 inactivated vaccines (P < 0.05). CONCLUSIONS: This is the first study to analyze the actual status of hospitals as COVID-19 vaccination clinics in China. The hospital has focused on vaccinating citizens and the initial rollout of vaccines to ensure any safety issues are identified. More citizens are willing to vaccinate in hospitals because of the uncertain safety of the available vaccines and adverse reactions. The good news is that vaccine-related severe adverse events have not been found in the hospital vaccination clinic. The Safety of BBIBP-CorV and CoronaVac is relatively high.
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Vacinas contra COVID-19 , COVID-19 , Humanos , Vacinas contra COVID-19/efeitos adversos , COVID-19/epidemiologia , COVID-19/prevenção & controle , Estudos Transversais , China/epidemiologia , Hospitais , Vacinas de Produtos Inativados , Vacinação/efeitos adversosRESUMO
The effects of twelve different pre-drying and drying methods on the chemical composition in the pericarp and kernel of Amomum tsao-ko were studied. The volatile components were isolated from the samples by simultaneous distillation and extraction and analyzed by gas chromatography-mass spectrometry (GC-MS). Sixty and thirty-eight compounds were identified from pericarp and kernel, respectively, and the main constituents were oxygenated monoterpenes. These compounds were not only significantly affected by pre-drying and drying methods but also varied in content due to different tissue locations. The total volatile content of pericarp varied from 0.70 to 1.55%, with the highest obtained by microwave-dried samples (150 W) and the lowest in freeze-dried samples. The total volatile content of the kernel varied from 6.11 to 10.69%, with the highest content obtained during sun drying (SD) and the lowest content in samples treated with boiling water for 2 min. Oxygenated monoterpenes were the highest compounds in pericarp and kernel, which were also the most affected by drying methods. The highest content of oxygenated monoterpenes in the pericarp (0.77%) could be obtained by boiling water treatment for 5 min, and the highest content of oxygenated monoterpenes in the kernel (7.48%) could be obtained by SD. Additionally, the main components such as 1,8-cineole, 2-carene, (Z)-citral, nerolidol, (Z)-2-decenal, (E)-2-dodecenal, citral, (E)-2-octenal, 4-propylbenzaldehyde, and phthalan showed remarkable variations in pre-drying and drying methods.
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Fraud in herbal medicines (HMs), commonplace throughout human history, is significantly related to medicinal effects with sometimes lethal consequences. Major HMs fraud events seem to occur with a certain regularity, such as substitution by counterfeits, adulteration by addition of inferior production-own materials, adulteration by chemical compounds, and adulteration by addition of foreign matter. The assessment of HMs fraud is in urgent demand to guarantee consumer protection against the four fraudulent activities. In this review, three analysis platforms (targeted, non-targeted, and the combination of non-targeted and targeted analysis) were introduced and summarized. Furthermore, the integration of analysis technology and chemometrics method (e.g., class-modeling, discrimination, and regression method) have also been discussed. Each integration shows different applicability depending on their advantages, drawbacks, and some factors, such as the explicit objective analysis or the nature of four types of HMs fraud. In an attempt to better solve four typical HMs fraud, appropriate analytical strategies are advised and illustrated with several typical studies. The article provides a general workflow of analysis methods that have been used for detection of HMs fraud. All analysis technologies and chemometrics methods applied can conduce to excellent reference value for further exploration of analysis methods in HMs fraud.
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Quimiometria , Plantas Medicinais , Fraude , Humanos , TecnologiaRESUMO
Polygonati Rhizoma was first recorded in Mingyi Bielu(《名医别录》) as both medicine and food due to its high edible and medicinal values.However,there is no systematic textual research on its use as medicine and food. Polygonati Rhizoma and Polygonati Odorati Rhizoma show similar morphology,so they are often confused.Clematis apiifolia and Polygonatum odoratum are often regarded as the original plants of Polygonati Odorati Rhizoma. By reviewing the related records in Chinese herbal books of the past dynasties,this paper aimed to clarify the relationship between Polygonati Rhizoma,C.apiifolia and P.odoratum,trace the historical evolution of Polygonati Rhizoma as medicine and food from the name,harvesting and processing,property,flavor and meridian tropism,efficacy and indications,edible and medicinal records,and contraindications,and summarize its application in ethnic medicine,in order to inherit and develop the ethnic medicine. The findings demonstrated that the name of Polygonati Rhizoma and its synonyms were derived from its pictogram,function,and place of origin,containing a wealth of myth implication and Taoism thought.Polygonati Rhizoma,C.apiifolia and P.odoratum are three species,different from the conclusions in previous textual research. The seedlings,flowers,seeds,and rhizomes of Polygonati Rhizoma all could be used for edible and medicinal purposes,with its edible records exceeding the medicinal records. There were 22 medical books from the ethnic minority groups such as The Annals of National Medicine in Yunnan,Zhongguo Minzu Yaozhi Yao,and Dictionary of Chinese Ethnic Medicine recording the knowledge and application of 12 species in Polygonatum by 26 ethnic minorities.Due to their different living environments,lifestyles,and cultural customs,ethnic minorities have formed their unique medical cultures.
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Tsaoko Fructus is a type of food with the homology of medicine and food,and has a long history of cultivation and application in China. With the deepening of the development and utilization of Tsaoko Fructus,its economic value has appeared obviously,and relevant industries have great potential,with an important role in poverty alleviation in mountainous areas. However,the plants source of Tsaoko Fructus are confused in the process of actual production and resource utilization,and there is a lack of systematic report about the origin of varieties and medicinal history. The paper focused on a textual research for its names,plant sources,changes of the genuine producing areas and traditional efficacy through consulting the herbal works and the analysis of modern literature. The results showed that the medicine of Tsaoko Fructus was first recorded in ancient literatures of the Song dynasty,and there were many aliases and synonyms of the herb, with a great difference between ancient and modern times. In modern records,the medicinal alias names such as Hongcaoguo,Tucaoguo,Caoguoren are similar with the Chinese name of Caoguo,but they are not the same kind of plant and shall be distinguished. In the Ming dynasty,variety and source of the herb was complicated,and it was often recorded as the same class of medicinal materials with Amomi Fructus Rotundus and Alpiniae Katsumadai Semen,until it was listed as a class of medicinal material and distinguished from confounding medicines in the Qing Dynasty. The prescriptions containing Tsaoko Fructus include Caoguoyin,Caoguosan,Caoguowan,Caoguoshushui. Tsaoko Fructus could be used as medicine with peel or only kernel according to different diseases,and mainly processed with water or wine. In addition,there are other processing methods,such as frying,salt-processing, ginger- processing,simmering flour. Ancient literatures have basically the same records on properties,efficacies and indications of Tsaoko Fructus,considering it was warm in nature with the effect in relieving vomiting,eliminating food,intercepting malaria,expelling phlegm. This study provided a theoretical basis for its origin,quality control and resource development and utilization.
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Polygonatum plants are perennial plants of Liliaceae. There are about 60 species reported at home and abroad,32 species in China,mainly distributed in the north temperate zone. Their main chemical components are steroidal saponins,polysaccharides,flavonoids,alkaloids,etc. They have anti-aging,anti-tumor,immunomodulation,antibacterial,antiviral,hypoglycemic and blood lipid effects. With the development of health industry,Polygonati Rhizome used as medicine and food has attracted great attention in recent years,and has become a research hotspot. However,the material basis of its efficacy is unclear and the product quality is uneven,which seriously limited the rapid upgrading of the industry. This review summarizes Polygonatum plants system classification,the chemical composition and pharmacological activity to provide theoretical basis for the development and utilization of Polygonatum plants.
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Compostos Fitoquímicos/farmacologia , Polygonatum/química , China , Compostos Fitoquímicos/química , Plantas Medicinais/química , Rizoma/químicaRESUMO
The Janus kinases (JAKs) consist of four similar tyrosine kinases and function as key hubs in the signaling pathways that are implicated in both innate and adaptive immunity. Among the four members, JAK3 is probably the more attractive target for treatment of inflammatory diseases because its inhibition demonstrates the greatest immunosuppression and most profound effect in the treatment of such disorders. Although many JAK3 inhibitors are already available, certain shortcomings have been identified, mostly acquired drug resistance or unwanted side effects. To discover and identify new promising lead candidates, in this study, the structure of JAK3 (3LXK) was obtained from the Protein Data Bank and used for simulation modeling and protein-ligand interaction analysis. The ~36,000 Chinese herbal compounds obtained from TCM Database@Taiwan were virtually screened by AutoDock Vina docking program and filtered with Lipinski's Rules and ADME/T virtual predictions. Because of high occurrence of fake hits during docking, we selected 12 phytochemicals which have demonstrated modulating JAKs expressions among the top 50 chemicals from docking results. To validate whether these compounds are able to directly mediate JAK3 kinase, we have investigated the inhibitory activity using enzymatic activity assays, western blot, and HEK 293 cell STAT5 transactivity assays. The molecular analysis included docking and molecular dynamics (MD) simulations in order to investigate structural conformations and to explore the key amino acids in the interaction between JAK3 kinase and its putative ligands. The results demonstrated that Cryptotanshinone, Icaritin, and Indirubin exhibited substantial inhibitory activity against JAK3 kinase in vitro. The results also provide binding models of the protein-ligand interaction, detailing the interacting amino acid residues at the active ATP-binding domains of JAK3 kinase. In conclusion, our work discovered 3 potential natural inhibitors of JAK3 kinase and could provide new possibilities and stimulate new insights for the treatment of JAK3-targeted diseases.
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Polygonatum plants are perennial plants of Liliaceae. There are about 60 species reported at home and abroad,32 species in China,mainly distributed in the north temperate zone. Their main chemical components are steroidal saponins,polysaccharides,flavonoids,alkaloids,etc. They have anti-aging,anti-tumor,immunomodulation,antibacterial,antiviral,hypoglycemic and blood lipid effects. With the development of health industry,Polygonati Rhizome used as medicine and food has attracted great attention in recent years,and has become a research hotspot. However,the material basis of its efficacy is unclear and the product quality is uneven,which seriously limited the rapid upgrading of the industry. This review summarizes Polygonatum plants system classification,the chemical composition and pharmacological activity to provide theoretical basis for the development and utilization of Polygonatum plants.
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China , Compostos Fitoquímicos , Química , Farmacologia , Plantas Medicinais , Química , Polygonatum , Química , Rizoma , QuímicaRESUMO
Colorectal cancer (CRC) is one of the most common malignancies and most frequent cause of cancer death worldwide. The activation of both NF-κB and STAT3 signaling and the crosstalk between them play an important role in colorectal tumor. Helicteres angustifolia L. is a type of commonly used Chinese medicinal herb and possesses a wide variety of biological activities. In the present study, we investigate the effects of three triterpenes from H. angustifolia (HT) such as helicteric acid (HA), oleanic acid (OA), and betulinic acid (BA), on inhibiting CRC progression. Our results showed that HT extracts could decrease proliferation and induce apoptosis in HT-29 colorectal cancer cells. Moreover, HT extracts could suppress LPS-triggered phosphorylation of IKK, IκB, and NF-κB, attenuate IL-6-induced phosphorylation of JAK2 and STAT3, and suppress the expression of c-Myc, cyclin-D1, and BCL-xL, the downstream gene targets of NF-κB and STAT3. Therefore, HT extracts showed potent therapeutic and antitumor effects on CRC via inhibiting NF-κB and STAT3 signaling.
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Aminopyrine (AMP) has been frequently detected in the aquatic environment. In this study, the transformation mechanism of AMP by free available chlorine (FAC) oxidation was investigated. The results showed that FAC reacted with AMP rapidly, and a 74% elimination was achieved for 1.30 µM AMP after 2 min at 14.08 µM FAC dose. AMP chlorination was strongly pH-dependent, and its reaction included second- and third-order kinetic processes. Three active FAC species, including chlorine monoxide (Cl2O), molecular chlorine (Cl2), and hypochlorous acid (HOCl), were observed to contribute to AMP degradation. The intrinsic rate constants of each FAC species with neutral (AMP0) and cation (AMP+) species were obtained by kinetic fitting. Cl2O exhibited the highest reactivity with AMP0 (kAMP0, Cl2O = (4.33 ± 1.4) × 109 M-1s-1). In addition, Cl2 showed high reactivity (106-107 M-1s-1) in the presence of chloride, compared with HOCl (kAMP+, HOCl = (5.73 ± 0.23) × 102 M-1s-1, kAMP0, HOCl = (9.68 ± 0.96) × 102 M-1s-1). At pH 6.15 and 14.08 µM FAC dose without chloride addition, the contribution of Cl2O reached to the maximum (33.3%), but in the whole pH range, HOCl was the main contributor (>66.6%) for AMP degradation. The significance of Cl2 was noticeable in water containing chloride. Moreover, 11 transformation products were identified, and the main transformation pathways included pyrazole ring breakage, hydroxylation, dehydrogenation, and halogenation.
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Aminopirina/química , Cloro/química , Poluentes Químicos da Água/química , Compostos Clorados/química , Halogenação , Concentração de Íons de Hidrogênio , Hidroxilação , Ácido Hipocloroso/química , Cinética , Oxirredução , Purificação da Água/métodosRESUMO
Objective: To develop a method for separation and purification of triterpenoids from Helicteres angustifolia by highspeed countercurrent chromatography( HSCCC). Methods: The ethyl acetate extract of Helicteres angustifolia were separated by two-step HSCCC. The structures of the target compounds were identified by ESI-MS and1H-NMR and characterized by FTIR. Results: Six compounds were isolated and prepared from ethyl acetate extract of Helicteres angustifolia,and identified as methyl helicterilate( 1),methyl helicterate( 2),helicterilic acid( 3),helicteric acid( 4),betulic acid( 5),oleanolic acid( 6). The purity of the chemical constituents were determined by HPLC,and the mass fraction was more than 95. 0%,respectively. Conclusion: This method is suitable for the separation and preparation of triterpenoids from Helicteres angustifolia,which is rapid,high purity and high yield.
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Malvaceae , Cromatografia Líquida de Alta Pressão , Distribuição Contracorrente , Espectroscopia de Ressonância Magnética , Triterpenos Pentacíclicos , Extratos Vegetais , Triterpenos , Ácido BetulínicoRESUMO
Objective: To establish the HPLC fingerprint method of Solanum nigrum fruit for its identification and quality evaluation. Methods: The analysis was carried out by Agilent ZORBAX SB-C18column( 150 mm × 4. 6 mm,5 µm),and eluted with mobile phase containing of acetonitrile-0. 3% phosphoric acid in a gradient mode. The temperature of column was 25 â,the flow rate was 1. 0m L / min, the detection wavelength was set at 205 nm, the injection volume was 10 µL. The similarity evaluation system for chromatographic fingerprint of TCM( version 2004A) was used to calculate the similarity degree of the HPLC fingerprint of Solanum nigrum fruit. . Results: The HPLC fingerprint of ten batches Solanum nigrum fruit was established with twelve common peaks. Two characteristic peaks included solasonine and solamargine were confirmed. Conclusion: The results indicate that establishing HPLC fingerprint of Solanum nigrum fruit can provide more comprehensive reference for identification and quality evaluation of Solanum nigrum fruit
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Cromatografia Líquida de Alta Pressão , Solanum nigrum , Medicamentos de Ervas Chinesas , Frutas , Controle de Qualidade , Alcaloides de SolanáceasRESUMO
Fascin actin-bundling protein 1 (FSCN1) plays significant roles in biological processes such as tumor cell invasion and metastasis. However, little is known about prognostic value of FSCN1 in non-small cell lung cancer (NSCLC). FSCN1 mRNA and protein expression were detected by real-time PCR and Western blot in NSCLC tissues and paired adjacent normal lung tissues. Furthermore, the association of FSCN1 protein expression with clinicopathological characteristics including the survival was explored in 156 NSCLC patients. In our results, FSCN1 mRNA and protein expression were obviously higher in NSCLC tissues than in normal lung tissues. High levels of FSCN1 protein were positively correlated with status of differentiated degree, clinical stage, N classification, and M classification in NSCLC. Meanwhile, higher FSCN1 protein expression was significantly associated with poor overall survival in patients with NSCLC. Multivariate analyses showed that increased FSCN1 protein expression was a poor independent prognostic biomarker for NSCLC patients. In conclusions, FSCN1 plays an important role on NSCLC progression and prognosis and may serve as a convictive prognostic biomarker for NSCLC patients.
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Biomarcadores Tumorais/biossíntese , Carcinoma Pulmonar de Células não Pequenas/metabolismo , Carcinoma Pulmonar de Células não Pequenas/patologia , Proteínas de Transporte/biossíntese , Neoplasias Pulmonares/metabolismo , Neoplasias Pulmonares/patologia , Proteínas dos Microfilamentos/biossíntese , Adulto , Idoso , Feminino , Humanos , Masculino , Pessoa de Meia-IdadeRESUMO
OBJECTIVE: To investigate the chemical constituents of Rubus alceaefolius. METHODS: Nine compounds were isolated and purified from the petroleum ether extract of 95% alcohol extract of Rubus alceaefolius by repeated column chromatography on silica, Sephadex LH-20 and structurally identified by spectral analysis. RESULTS: The compounds were identified as chrysophanol(1), physcion (2), ß-sitosterol(3), 3-oxotirucalla-7, 24-dien-21-oic acid(4), myricadiol(5), 19-α-hydroxy-3-acetyl-ursolic acid(6), N-benzoylphenylalaninyl-N-benzoylphenylalaninate(7), aurantiamide acetate(8) and euscaphic acid(9). CONCLUSION: Compounds land 4~8 are isolated from this plant for the first time, and compounds 4 - 8 are found in plants of Rubus genus for the first time.
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Compostos Fitoquímicos/química , Extratos Vegetais/química , Rubus/química , Dipeptídeos , Emodina/análogos & derivados , Compostos Fitoquímicos/isolamento & purificação , Sitosteroides , Solventes , TriterpenosRESUMO
OBJECTIVE: To establish the HPLC fingerprint of Clerodendrum lindleyi in order to provide the basis for its quality standard. METHODS: The chromatographic fingerprint was obtained with Angilent Zorbax C18 (250 mm x 4.6 mm, 5 µm) column and gradiently eluted with acetonitrile-0.1% phosphoric acid solution. The column temperature was maintained at 35 degrees C. The flow rate was 1.0 mL/min and the detection wavelength was 327 nm. RESULTS: HPLC fingerprint of Clerodendrum lindleyi was established and 21 common peaks from 11 batches of samples were found. CONCLUSION: The method has good precision, stability and repeatability, which can provide reliable basis for quality evaluation of Clerodendrum lindleyi.
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Cromatografia Líquida de Alta Pressão , Clerodendrum/química , Medicamentos de Ervas Chinesas/química , Medicamentos de Ervas Chinesas/normas , Controle de QualidadeRESUMO
A simultaneous determination method of 14 multi-class pharmaceuticals using solid-phase extraction (SPE) followed by high-performance liquid chromatography-tandem mass spectrometer (HPLC-MS/MS) was established to measure the occurrence and distribution of these pharmaceuticals in tap water and a drinking water treatment plant (DWTP) in Beijing, China. Target compounds included seven anti-inflammatory drugs, two antibacterial drugs, two lipid regulation drugs, one antiepileptic drug, and one hormone. Limits of detection (LODs) and limits of quantitation (LOQs) ranged from 0.01 to 1.80 ng/L and 0.05 to 3.00 ng/L, respectively. Intraday and inter-day precisions, recoveries of different matrices, and matrix effects were also investigated. Of the 14 pharmaceutical compounds selected, nine were identified in tap water of Beijing downtown with the concentration up to 38.24 ng/L (carbamazepine), and the concentration levels of detected pharmaceuticals in tap water (<5 ng/L for most pharmaceuticals) were lower than previous studies in other countries. In addition, ten and six pharmaceuticals were measured in raw water and finished water at the concentration ranged from 0.10 to 16.23 and 0.13 to 17.17 ng/L, respectively. Five compounds were detected most frequently in DWTP, namely antipyrine, carbamazepine, isopropylantipyrine, aminopyrine, and bezafibrate. Ibuprofen was found to be the highest concentration pharmaceutical during DWTP, up to 53.30 ng/L. DWTP shows a positive effect on the removal of most pharmaceuticals with 81.2-99.5 % removal efficiencies, followed by carbamazepine with 55.4 % removal efficiency, but it has no effect for removing ibuprofen and bezafibrate.