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1.
Inorg Chem ; 2020 May 15.
Artigo em Inglês | MEDLINE | ID: mdl-32410454

RESUMO

Good aqueous dispersibility of metal chalcogenide nanoclusters with an atomically precise structure is desirable to achieve tiny and uniform cluster-based "quantum dots". However, there are big challenges toward this goal, especially for the large-sized nanoclusters without covalently bonded organic ligands, because the strong electrostatic interactions between closely packed negatively charged nanoclusters and protonated organic amine templates in the crystal lattice impede the dispersion of cluster-based bulk crystalline samples. Here, we report two iso-structured crystalline metal chalcogenides composed of discrete supertetrahedral T4-MInS nanoclusters with the formulas of [M4In16S35]14- (denoted ISC-16-MInS, M = Zn and Fe), which adopt a sodalite-net loose-packing pattern in the crystal lattice and display superior dispersibility in water and some organic solvents as compared to other cases composed of the same type of nanoclusters with close-packing pattern. The dispersed T4-MInS nanoclusters were unexpectedly stabilized by adsorbing a certain number of H+ ions on surface S sites and simultaneously dropping partial surface S2- ions, instead of being surrounded by protonated organic amines, which was clearly verified by electrospray ionization mass spectrometry analysis. Notably, ISC-16-ZnInS behaves with superior performance on photodegradation of rhodamine B dye to ISC-16-FeInS. This is attributed to their difference in divalent-metal-directed separation efficiency of the photogenerated electrons and holes. This work holds great promise for the potential functional applications of uniformly dispersed semiconductor nanoclusters, such as cluster-based thin film devices, photoelectrodes, and photocatalysis.

2.
Nanoscale ; 12(16): 8875-8882, 2020 Apr 30.
Artigo em Inglês | MEDLINE | ID: mdl-32259173

RESUMO

BiVO4 has been widely used as a photoanode material, while the slow surface oxygen evolution reaction (OER) kinetics still severely hinders its performance. Here, an efficient bimetallic cocatalyst (named FeSnOS) was obtained by post-annealing a Fe/Sn-containing metal chalcogenide coordination compound to enhance the OER activity of BiVO4. The synergistic effect of Fe and Sn species in the amorphous FeSnOS cocatalyst efficiently lowers the interface impedance of the photoanode, reduces the electrochemical reaction overpotential, and promotes the surface OER dynamics. At the same time, a type-II heterojunction was constructed due to the process of post-annealing, which efficiently improves the bulk phase charge separation efficiency of the photoanode. The obtained optimal photoanode (named FeSnOS-BiVO4) shows a photocurrent density of 3.1 mA cm-2 at 1.23 V vs. the reversible hydrogen electrode, which is 3.4 times higher than that of the pristine BiVO4 photoanode, and its onset potential shifts negatively from 0.44 V to 0.25 V. This work presents a simple and effective method to build a bimetallic cocatalyst for improved photoelectrochemical performance, which extends the application of polymetallic metal chalcogenide complexes.

3.
J Am Chem Soc ; 142(14): 6649-6660, 2020 Apr 08.
Artigo em Inglês | MEDLINE | ID: mdl-32176486

RESUMO

Strong Mn-Mn coupling interactions (dipole-dipole and spin-exchange), predominantly determined by statistically and apparently short Mn···Mn distances in traditional heavily Mn2+-doped semiconductors, can promote energy transfer within randomly positioned and close-knit Mn2+ pairs. However, the intrinsic mechanism on controlling Mn2+ emission efficiency is still elusive due to the lack of precise structure information on local tetrahedrally coordinated Mn2+ ions. Herein, a group of Mn2+-containing metal-chalcogenide open frameworks (MCOFs), built from [Mn4In16S35] nanoclusters (denoted T4-MnInS) with a precise [Mn4S] configuration and length-variable linkers, were prepared and selected as unique models to address the above-mentioned issues. MCOF-5 and MCOF-6 that contained a symmetrical [Mn4S] core with a D2d point group and relatively long Mn···Mn distance (∼3.9645 Å) exhibited obvious red emission, while no room-temperature PL emission was observed in MCOF-7 that contained an asymmetric [Mn4S] configuration with a C1 point group and relatively short Mn···Mn distance (∼3.9204 Å). The differences of Mn-Mn dipole-dipole and spin-exchange interactions were verified through transient photoluminescent spectroscopy, electron spin resonance (ESR), and magnetic measurements. Compared to MCOF-5 and MCOF-6 showing a narrower/stronger ESR signal and longer decay lifetime of microseconds, MCOF-7 displayed a much broader/weaker ESR signal and shorter decay lifetime of nanoseconds. The results demonstrated the dominant role of distance-directed Mn-Mn dipole-dipole interactions over symmetry-directed spin-exchange interactions in modulating PL quenching behavior of Mn2+ emission. More importantly, the reported work offers a new pathway to elucidate Mn2+-site-dependent photoluminescence regulation mechanism from the perspective of atomically precise nanoclusters.

4.
Molecules ; 25(3)2020 Jan 31.
Artigo em Inglês | MEDLINE | ID: mdl-32023945

RESUMO

Farfarae Flos (FF) is the dried flower bud of Tussilago farfara L, which has antitussive, expectorant, and anti-inflammatory effects. However, little research on the main active composition of FF has been reported. The purpose of this study is to find the main active compounds responsible for the three pharmacological effects (i.e., antitussive, expectorant, and anti-inflammatory effects) of Farfarae Flos, based on the spectrum-effect relationship combined with chemometrics. First, this study uses the UPLC-QDA method to establish the chromatography fingerprint of Farfarae Flos, which is combined with chemometrics to analyze 18 batches of samples. Then, we study the antitussive, expectorant, and anti-inflammatory effects of Farfarae Flos. Finally, the spectrum-effect relationship between the fingerprint and the three pharmacological effects are studied by grey correlation analysis and partial least squares regression. The results show that four, four, and three main active constituents were found for the antitussive, expectorant, and anti-inflammatory pharmacological effects, respectively. In conclusion, we found the main active compounds corresponding to the main pharmacodynamic effects of Farfarae Flos. To our knowledge, this is the first time that spectrum-effect relationships in FF have been established using both raw and processed samples, which provides an experimental basis for further studies on the pharmacodynamic material basis of Farfarae Flos, as well as providing reference for the comprehensive evaluation of Farfarae Flos quality and the development of substitute resources.

5.
Glycoconj J ; 37(3): 373-394, 2020 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-32103424

RESUMO

Currently, the definitive diagnosis in breast cancer requires biopsy and histopathology, such the most effective markers are tissue-based. However, the advantages of saliva in collection and storage make it possible for assessing human pathology and contributing to the development of cancer-related biomarkers for clinical application. The present study validated alteration of salivary protein glycopatterns recognized by Bandeiraea simplicifolia lectin I (BS-I) in the saliva of patients with breast diseases using saliva microarrays, and the N/O-glycan profiles of their salivary glycoproteins isolated by the BS-I-magnetic particle conjugates from 259 female subjects (66 healthy volunteers (HV), 65 benign breast cyst or tumor patients (BB), 66 patients with breast cancer in stage I (BC-I) and 62 patients with breast cancer in stage II (BC-II)) were analyzed by MALDI-TOF/TOF-MS. The results showed that the expression level of galactosylated glycans recognized by BS-I was significantly increased in patients with breast cancer compared with HV (p < 0.05). Totally, there were 11/10, 10/19, 7/24 and 7/9 galactosylated N-/O-linked glycans were identified and annotated from the pooled salivary samples of HV, BB, BC-I and BC-II, respectively. One galactosylated N-glycan peak (m/z 2773.977), and 4 galactosylated O-glycan peaks (m/z 868.295, 882.243, 884.270 and 1030.348) were found only in BC-I. These findings could provide pivotal information on galactosylated N/O-linked glycans related to breast cancer, and promote the study of biomarkers for early-stage breast cancer based on precise alterations of galactosylated N/O-glycans in saliva.

6.
Anal Biochem ; 596: 113643, 2020 May 01.
Artigo em Inglês | MEDLINE | ID: mdl-32105738

RESUMO

The aim of this study is to establish a method for rapid screening of active ingredients targeting TNF-α from Chinese herbal medicines. Take Angelicae Pubescentis Radix (APR) as an example, surface plasma resonance technique was used to establish for screening small molecule inhibitors of TNF-α from APR extract. Then UPLC-MS/MS coupled with chemometric was used for quantitative and evaluate the differences of the candidate compounds bound to TNF-α in APR from different sources. In the experiment, TNF-α protein was fixed on the CM5 chip surface of biacore T200 biosensor by amino coupling. A series of small molecular compounds in APR were screened and six phenolic acid compounds had a strong affinity for TNF-α protein and could be used as TNF-α antagonists. In summary, the targeted drug screening method for TNF-α protein based on SPR technology established in this study can be used to screen anti-TNF-α small molecule inhibitors. UPLC-MS/MS can accurately quantify 15 active ingredients, which provides reliable experimental data and new research ideas for targeted drug research on TNF-α protein.

7.
J Surg Res ; 246: 442-449, 2020 02.
Artigo em Inglês | MEDLINE | ID: mdl-31635836

RESUMO

BACKGROUND: MicroRNA (miRNA)-382-5p functions as an oncogenic miRNA in breast cancer. MXD1 was demonstrated to be one of its direct targets. However, the involvement of miRNA-382-5p/MXD1 axis in breast cancer remains unknown. The aim of this study was to investigate the expression pattern, clinical significance, and potential functions of miRNA-382-5p/MXD1 axis in breast cancer. MATERIALS AND METHODS: Quantitative polymerase chain reaction was performed to detect the expression levels of miRNA-382-5p and MXD1 messenger RNA (mRNA) in 96 pairs of breast cancer and matched noncancerous breast tissue samples from the same patients. Relationships between miRNA-382 expression, MXD1 expression, and combined miRNA-382-5p and MXD1 expression, and various clinicopathological characteristics of breast cancer were statistically evaluated, and their roles in breast cancer cell proliferation and invasion were also examined. RESULTS: Compared with noncancerous breast tissues, miRNA-382-5p expression was upregulated but MXD1 mRNA expression was downregulated in breast cancer tissues (both P < 0.01). High miRNA-382 expression, MXD1 expression, and combined miRNA-382-5p and low MXD1 expression were significantly associated with advanced tumor stage and the presence of lymph node metastasis (all P < 0.05). Overexpression of miRNA-382-5p dramatically reduced MXD1 mRNA and protein expression levels in breast cancer cells. miRNA-382-5p upregulation markedly enhanced breast cancer cell proliferation and invasion, while its downregulation inhibited these malignant phenotypes of breast cancer cells in vitro. Notably, overexpressed MXD1 reversed the effects of upregulated miRNA-382-5p on cell proliferation and invasion in vitro. CONCLUSIONS: The dysregulation of miRNA-382-5p-MXD1 axis may be involved in the development and aggressive progression of breast cancer. miRNA-382-5p may target MXD1, leading to cell invasion and proliferation in breast cancer cells in vitro, implying its potentials as a therapeutic target for this type of cancer.


Assuntos
Fatores de Transcrição de Zíper de Leucina e Hélice-Alça-Hélix Básicos/genética , Neoplasias da Mama/genética , Regulação Neoplásica da Expressão Gênica , MicroRNAs/metabolismo , Proteínas Repressoras/genética , Fatores de Transcrição de Zíper de Leucina e Hélice-Alça-Hélix Básicos/metabolismo , Mama/patologia , Neoplasias da Mama/patologia , Proliferação de Células/genética , Progressão da Doença , Regulação para Baixo , Feminino , Humanos , Células MCF-7 , Pessoa de Meia-Idade , Invasividade Neoplásica/genética , RNA Mensageiro/metabolismo , Proteínas Repressoras/metabolismo
8.
Nanoscale ; 12(2): 772-784, 2020 Jan 02.
Artigo em Inglês | MEDLINE | ID: mdl-31830183

RESUMO

The direct electroreduction of CO2 to ratio-tunable syngas (CO + H2) is an appealing solution to provide important feedstocks for many industrial processes. However, low-cost, Earth-abundant yet efficient and stable electrocatalysts for composition-adjustable syngas have still not been realized for practical applications. Herein, new hierarchical 0D/2D heterostructures of SnO2 nanoparticles (NPs) confined on CuS nanosheets (NSs) were designed to enable CO2 electroreduction to a wide-range syngas (CO/H2: 0.11-3.86) with high faradaic efficiency (>85%), remarkable turnover frequency (96.12 h-1) and excellent durability (over 24 h). Detailed experimental characterization studies together with theoretical calculations manifest that the ascendant catalytic performance is not only attributed to the heterostructure of ultrasmall SnO2 NPs homogeneously confined on ultrathin CuS NSs, which endows the maximum exposure of active sites and faster charge transfer, but is also accounted by the strong interaction between well-defined SnO2 and CuS interfaces, which modulated reaction free-energies of reaction intermediates and hence improved the activity of CO2 electroreduction to highly ratio-tunable syngas. This work provides a better understanding and a new strategy for intermediate regulation by interface engineering of hereostructures for CO2 reduction and beyond.

9.
J Phys Chem A ; 123(45): 9791-9799, 2019 Nov 14.
Artigo em Inglês | MEDLINE | ID: mdl-31633930

RESUMO

Recent guided ion beam experiments have revealed interesting reaction dynamics of the HBr+ + CO2 → HOCO+ + Br· reaction under different conditions. The hypothesis is that the predominant reaction mechanism depends on the collision energy between two reactants, the angular momentum of HBr+, and the spin-orbit coupling state of the system. The potential energy profile of the HBr+ + CO2 → HOCO+ + Br· reaction is studied in this research to lay the groundwork for an ab initio molecular dynamics simulation. First, a benchmark potential energy profile of this reaction is identified using coupled-cluster theory extrapolated to the complete basis set limit. A transition state connecting the previously reported intermediates is found, making the potential energy surface of the HBr+ + CO2 → HOCO+ + Br· reaction double-welled. Second, various single reference ab initio methods are compared with the benchmark potential energy profile to search for the most suitable ab initio method for the dynamics simulation. Two combinations of double-ζ basis sets (with effective core potentials) with MP2 and density functional theory have been identified to accurately represent the potential energy profile of this reaction.

10.
Inorg Chem ; 58(18): 12415-12421, 2019 Sep 16.
Artigo em Inglês | MEDLINE | ID: mdl-31483642

RESUMO

Many strategies to optimize molybdenum selenide based electrocatalysts for hydrogen evolution reaction (HER) have been explored; however, the modulation of molybdenum selenide on the molecular scale remains an ongoing challenge. Here, we synthesized a new molecular HER electrocatalyst based on a molybdenum-selenium cluster (Mo3Se13) and further realized its modulation by precise sulfur substitution at the molecular level to enhance the HER activity. The density functional theory (DFT) calculations demonstrated that the substituted sulfur could promote the hydrogen adsorption process and thus improve the HER performance. This work not only realizes the selective replacement of the bridging selenium atom with a sulfur atom in the molybdenum-selenium cluster for the first time but also provides a precise model for illustrating the structure-property relationship in electrocatalysis on the molecular level.

11.
Mar Pollut Bull ; 149: 110569, 2019 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-31546109

RESUMO

This study involved an assessment of the levels of microplastic pollution in seven small-scale estuaries in Shanghai for the first time. The abundance of microplastics ranged from 13.53 ±â€¯4.6 to 44.93 ±â€¯9.41 particles L-1, with a mean abundance of 27.84 ±â€¯11.81 particles L-1. Microplastics collected from samples were classified into four types (fiber, film, granule, and fragment), and granules were the most abundant type. Up to 99.5% of microplastics were <2 mm in diameter. The microplastics had a variety of colors, with black being the dominant color. Polypropylene (37.5%) and polyethylene (50%) were the main types of microplastic component validated. Our study showed severe microplastic pollution in small-scale estuaries, and the associated rivers need urgent attention for microplastic pollution prevention.


Assuntos
/análise , Poluentes Químicos da Água/análise , China , Cor , Monitoramento Ambiental , Estuários , Polietileno/análise , Polipropilenos/análise , Rios
12.
Anal Chem ; 91(16): 10663-10671, 2019 Aug 20.
Artigo em Inglês | MEDLINE | ID: mdl-31353882

RESUMO

Glycosphingolipids (GSLs) are ubiquitous glycoconjugates of cell membranes. Identification of unknown GSL-glycan structures is still a major challenge. To address this challenge, we developed a novel strategy for analysis of GSL-glycans from cultured cells based on a lectin microarray that can directly detect and reveal glycopatterns of GSL extracts without the need for glycan release. There were six steps to perform the analysis of GSL-glycans: (i) extraction of GSLs from cell pellets, (ii) quantification of GSL-glycans using orcinol-sulfuric acid reaction, (iii) preparation of lyso-GSLs by using sphingolipid ceramide N-deacylase, (iv) fluorescence labeling of lyso-GSLs, (v) detection by a lectin microarray, (vi) data acquisition and analysis. Simultaneously, a supplementary verification analysis for GSL-glycans was performed by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry. Optimized experimental conditions, which consisted of the blocking buffer, incubation buffer, and appropriate GSL concentration, were investigated by analyzing the glycopatterns of a standard ganglioside (GM1a) via lectin microarray. The analysis of GSL-glycans from human hepatocarcinoma cell lines (MHCC97L, MHCC97H, and HCCLM3) showed that there were 27 lectins (e.g., WFA, MAL-II, and LTL) to give significantly different signals compared with a normal human liver cell line (HL-7702), indicating up- and/or down-regulations of corresponding glycopatterns such as α1-2 fucosylation and α2-3 sialylation, and changes of certain glycostructures such as Galß1-3GalNAcß1-4(NeuAcα2-3)Galß1-4Glc:Cer and GalNAcα1-3(Fucα1-2)Galß1-3GlcNAcß1-3Galß1-4Glc:Cer. The lectin microarray analysis of lyso-GSLs labeled by fluorescence has proven to be credible, which can provide the glycopatterns and detailed linkage information on GSL-glycans.

13.
Dalton Trans ; 48(29): 10799-10803, 2019 Aug 07.
Artigo em Inglês | MEDLINE | ID: mdl-31263815

RESUMO

Enlarging the openess of chalcogenide frameworks is of significance for functionalizing semiconducting open frameworks, which are usually limited by their own interpenetration due to the rigid clusters and monotonous linkers. Herein, we report two zeolite-like chalcogenide open frameworks constructed from unusual defective supertetrahedral clusters and various kinds of linkers. Both the structures exhibit impressive architecture and high extra-framework volume ratios.

14.
Chem Commun (Camb) ; 55(56): 8146-8149, 2019 Jul 18.
Artigo em Inglês | MEDLINE | ID: mdl-31240283

RESUMO

Herein, we report a simple, yet highly effective approach for constructing a new type of sub-nanoscale ZnS/ZnO heterojunction (∼2-4 nm) with highly rich interfaces by photoetching hybrid Zn-S-O molecular clusters. The obtained ZnS/ZnO heterojunctions with ZnS spheres decorated with ultrasmall amorphous ZnO dots exhibit superior photocatalytic performance (∼94.0 µmol g-1 h-1), compared to nanoscale homologous samples obtained via conventional heat treatment (∼17.0-21.4 µmol g-1 h-1). Such a light-triggered molecular-cluster-to-heterojunction strategy provides a synthetic approach to building other sub-nanoscale hetero-structured materials for further promoting the catalytic-related applications.

15.
Chem Commun (Camb) ; 55(45): 6357-6360, 2019 May 30.
Artigo em Inglês | MEDLINE | ID: mdl-31065633

RESUMO

Here we report two new metal-chalcogenide open frameworks (MCOFs) with large-sized supertetrahedral clusters bridged by an accessible single-cuprous ion via a multivalent mixed-metal strategy. Such Cu-rich semiconductor MCOFs have been investigated for the first time for nonenzymatic detection of glucose, and display good sensitivity and stability.


Assuntos
Calcogênios/química , Cobre/química , Glucose/análise , Estruturas Metalorgânicas/química
16.
Dalton Trans ; 48(22): 7537-7540, 2019 Jun 14.
Artigo em Inglês | MEDLINE | ID: mdl-31066399

RESUMO

Reported here are three new metal chalcogenide open frameworks built from supertetrahedral [In35S52O8] (denoted as T5-InOS or o-T5) and [In10S20] (denoted as T3-InS) nanoclusters of different sizes and compositions via co-assembly and/or hybrid assembly modes. Such a set of cluster-based superlattices with dia topological structures clearly exhibit quantum size effects and electronic coupling interaction of adjacent nanoclusters, which can effectively explain that the band gap of the T3-(o-T5) hybrid-assembled material lies in the middle of T3-T3 and (o-T5)-(o-T5) co-assembled materials.

17.
Nanoscale ; 11(16): 7588-7594, 2019 Apr 23.
Artigo em Inglês | MEDLINE | ID: mdl-30964473

RESUMO

Two-dimensional (2D) nanostructure engineering and surface modification with functional groups are of great importance to anode materials for rechargeable lithium-ion batteries. Herein, stacked NiO nanosheets@carbon (denoted as NiO@C) and 3 nm-ultrathin NiO nanosheets@functionalized carbon with surface functional groups NO3-, CO32-, OH-, and COOH- (denoted as NiO@FC) were prepared via a facile one-pot reaction and topotactic conversion. Specifically, NiO@FC exhibits excellent lithium storage performance: the capacity of NiO@FC is 489.2 mA h g-1, higher than that of NiO@C (1018.7 mA h g-1 at 0.2 A g-1), and maintains a capacity of 1133 mA h g-1 after 800 cycles, which exceed that of all previously reported NiO anodes. The enhanced lithium storage performance is attributed to the sufficient void space, which offers buffer space for volume change and speeds up the diffusion of Li+ ions. In addition, the surface functional groups were proved to not only hinder the agglomeration of nanosheets but also further donate active sites and improve storage capacity. These advantageous features achieved by designing such a stacked structure with functionalized carbon modification provide a promising strategy for the preparation of high-performance anode materials and other 2D functional materials.

18.
Inorg Chem ; 58(6): 3582-3585, 2019 Mar 18.
Artigo em Inglês | MEDLINE | ID: mdl-30793596

RESUMO

High-degree connectivity of clusters in open-framework chalcogenide semiconductors conceptually facilitates electron mobility between clusters; however, no direct evidence was obtained to prove the prediction because of the shortage of suitable structure models among such systems. Herein, two open-framework chalcogenides built from the same types of heterometallic P2-CuInSnS clusters but with different spatial connectivities of clusters were obtained, in which 3-connected clusters are assembled into a 3D framework with SrSi2 topology (MCOF-1) and 4-connected clusters (µ4-P2) are arranged into diamond topology (MCOF-2). Compared to MCOF-1, MCOF-2 exhibits a relatively rapid photocurrent response, good reproducibility, and high electrocatalytic oxygen reduction reaction activity. This work substantially demonstrates that cluster-based chalcogenide frameworks with higher-degree cluster connectivity possess faster electron-transport efficiency between adjacent clusters relative to low-connected ones with the same building units.

19.
J Phys Chem A ; 123(11): 2203-2210, 2019 Mar 21.
Artigo em Inglês | MEDLINE | ID: mdl-30794408

RESUMO

The study of microsolvation provides a deeper understanding of solvent effects on reaction dynamics. Here, the properties of the SN2 reaction of hydrated chloride with methyl iodide are investigated by direct dynamics simulations, and how the solute-solvent interactions and the basicity of nucleophiles can profoundly affect the atomic level dynamics is discussed in detail. The results show that the direct-rebound mechanism dominates the substitution reaction, and the roundabout mechanism, which prevails in the indirect unsolvated counterpart reaction, still accounts for a high proportion of the indirect mechanisms. The involvement of a solvent water molecule does not significantly reduce the cross section and rate constant compared to the unhydrated reaction at high collision energy. By varying solvated Cl- to F-, the dominant mechanisms are totally different and in contrast, the dynamics of water does not show much difference, and the departure of H2O tends to occur prior to the substitution reaction because of the facile breakage of the hydrogen bond at high collision energy.

20.
Inorg Chem ; 58(1): 31-34, 2019 Jan 07.
Artigo em Inglês | MEDLINE | ID: mdl-30550271

RESUMO

Reported here are two novel metal chalcogenide superlattices built from unusual supertetrahedral TO2-InSnS clusters. With regard to only one previously reported case of a TO2-InS-based 2D-layered structure, such a combination of In-Sn-S components is thought to be reasonable for leading to the first observation of 3D superlattices based on TO2-InSnS clusters. Besides, these title semiconducting materials also display good performance on the electrocatalytic oxygen reduction reaction.

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