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1.
J Chromatogr A ; 1721: 464844, 2024 Apr 26.
Artigo em Inglês | MEDLINE | ID: mdl-38547678

RESUMO

The highly conjugated and hydrophobic characteristics of microporous organic networks (MONs) have largely impeded their broad applications in sample pretreatment especially for the polar or ionic analytes. In this work, a novel uniform hollow shaped sulfonate group functionalized MON (H-MON-SO3H-2) was synthesized via the sacrificial template method for the efficient solid phase extraction (SPE) of sulfonamides (SAs) from environmental water, milk, and honey samples prior to HPLC analysis. H-MON-SO3H-2 exhibited large specific surface area, penetrable space, good stability, and numerous hydrogen bonding, electrostatic, hydrophobic and π-π interaction sites, allowing sensitive SPE of SAs with wide linear range (0.150-1000 µg L-1), low limit of detection (0.045-0.188 µg L-1), good precisions (intra-day and inter-day RSD < 7.3%, n = 5), large enrichment factors (95.7-98.5), high adsorption capacities (250.4-545.0 mg g-1), and satisfactory reusability (more than 80 times). Moreover, the established method was successfully applied to extract SAs from spiked samples with the recoveries of 86.1-104.3%. This work demonstrated the great potential of H-MON-SO3H-2 in the efficient SPE of trace SAs in complex environmental water and food samples and revealed the prospect of hollow MONs in sample pretreatment.


Assuntos
Antibacterianos , Mel , Antibacterianos/análise , Mel/análise , Extração em Fase Sólida/métodos , Cromatografia Líquida de Alta Pressão/métodos , Sulfanilamida/análise , Água/química , Sulfonamidas/análise
2.
J Chromatogr A ; 1715: 464625, 2024 Jan 25.
Artigo em Inglês | MEDLINE | ID: mdl-38171066

RESUMO

Endocrine disrupting chemicals (EDCs) are a typical class of natural or man-made endogenous hormone agonists or antagonists that can directly or potentially interfere with human endocrine system. However, it is still difficult to analyze trace EDCs directly from complex environment and food matrices. Therefore, the proper sample pretreatment is highly desired and the preparation of efficient adsorbents is of great challenge and importance. Herein, we report the facile one-pot solvothermal synthesis of Fe3O4 nanoparticle doped magnetic ß-cyclodextrin microporous organic network composites (MCD-MONs) for the magnetic solid phase extraction (MSPE) of four phenolic EDCs in water and food takeaway boxes prior to the high-performance liquid chromatography analysis. The sheet-like Fe3O4 doped MCD-MONs offered good magnetic property (16.5 emu g-1) and stability, and provided numerous hydrogen bonding, hydrophobic, π-π, and host-guest interaction sites for EDCs. Under the optimal experimental conditions, the established method was successfully verified with wide linear range (2.0-1000 µg L-1), low limits of detection (0.6-1.0 µg L-1), good precisions (intra-day and inter-day RSDs < 5.2 %, n = 3), large enrichment factors (88-98) and adsorption capacity (90.3-255.8 mg g-1), short extraction time (6 min), less adsorbent consumption (3 mg), and good reusability (at least 8 times) for EDCs. The proposed method was successfully applied to detect the trace EDCs in real samples with the recovery of 84.0-99.7 %. This work demonstrated the great potential of MCD-MONs for the efficient MSPE of trace EDCs from complex food takeaway boxes and water samples and uncovered the prospect of CD-based MONs in sample pretreatment.


Assuntos
Disruptores Endócrinos , beta-Ciclodextrinas , Humanos , Disruptores Endócrinos/análise , Água/química , Magnetismo/métodos , Cromatografia Líquida de Alta Pressão , Fenômenos Magnéticos , beta-Ciclodextrinas/química , Extração em Fase Sólida/métodos , Limite de Detecção
3.
Food Chem ; 443: 138559, 2024 Jun 15.
Artigo em Inglês | MEDLINE | ID: mdl-38280368

RESUMO

Cephalosporins (CEFs) are a class of widely used toxic antibiotics. Development of a rapid and sensitive method for detecting trace CEF residues in food samples is still challenging. Herein, we report preparation of an amide and carboxyl groups dual-functionalized core-shelled magnetic microporous organic network MMON-COOH-2CONH for efficient magnetic solid-phase extraction (MSPE) of CEFs from milk powder samples. Under optimal conditions, the established MMON-COOH-2CONH-MSPE-HPLC-UV method owns wide linear range (3-10000 µg kg-1), low limits of detection (1-3 µg kg-1), large enrichment factors (93.9-99.4), low adsorbent consumption (3 mg), and short extraction time (6 min). Synergistic extraction mechanisms of ionic bonding, hydrogen bonding, π-π, and hydrophobic interactions were elucidated by both theoretical density functional theory calculations and experimental data. This study confirms that preparation of dual-functionalized MMONs and introduction of ionic groups are feasible to promote MMONs application in sample pretreatment.


Assuntos
Amidas , Cefalosporinas , Magnetismo , Fenômenos Físicos , Extração em Fase Sólida/métodos , Cromatografia Líquida de Alta Pressão , Fenômenos Magnéticos , Limite de Detecção
4.
Food Chem ; 429: 136808, 2023 Dec 15.
Artigo em Inglês | MEDLINE | ID: mdl-37459710

RESUMO

A zwitterionic magnetic microporous organic network (MMON-SO3H-NH2) with numerous amino and sulfonic acid ion-pare binding sites was designed and synthesized for efficient magnetic solid-phase extraction (MSPE) of fluoroquinolones (FQs) from meat samples. The core-shell MMON-SO3H-NH2 offered large specific surface area, rapid magnetic responsiveness, good stability, and multiple binding sites for FQs. The density functional theory and independent gradient model evaluations confirmed hydrogen bonding, π-π and ion-pair interactions between MMON-SO3H-NH2 and FQs. Under the optimal conditions, the established MMON-SO3H-NH2-MSPE-HPLC-UV method gave wide linear range (0.15-1000 µg L-1), low limits of detection (0.05-4.5 µg L-1) and limits of quantitation (0.15-13 µg L-1), and high enrichment factors (82.1-99.6) using 3 mg of adsorbent. This work demonstrates that the preparation of zwitterionic MONs is an efficient way to promote the extraction performance of MONs for zwitterionic targets and provides an effective sample pretreatment method for enriching and monitoring FQs in complex food matrices.


Assuntos
Fluoroquinolonas , Extração em Fase Sólida , Fluoroquinolonas/análise , Cromatografia Líquida de Alta Pressão , Extração em Fase Sólida/métodos , Antibacterianos , Carne/análise , Fenômenos Magnéticos , Limite de Detecção
5.
BMC Nurs ; 22(1): 250, 2023 Jul 28.
Artigo em Inglês | MEDLINE | ID: mdl-37507706

RESUMO

OBJECTIVE: To translate the career success in nursing scale (CSNS) into Chinese and evaluate its psychometric properties. BACKGROUND: A lower sense of career success seriously affects the enthusiasm of nurses and increases their turnover rate. Therefore, an accurate assessment of the career success level of nurses is necessary. However, China does not have a professional tool for assessing the career success of nurses. METHODS: The stratified sampling method was used to recruit participants from 22 hospitals of different grades in 5 cities in China. A total of 650 and 348 subjects were selected for item analysis and reliability and validity tests, respectively, of the translated initial scale. RESULTS: The Chinese version of the CSNS (C-CSNS) with 33 items had good psychometric properties. Cronbach's α was 0.960, split-half reliability was 0.893, and ICC within two weeks was 0.981. Exploratory factor analysis extracted 5 common factors that explained 63.73% of the total variance, and confirmatory factor analysis supported acceptable construct validity. CONCLUSION: The C-CSNS has adequate construct validity and excellent psychometric properties and can be used for accurate assessment of nurses' career success. IMPLICATIONS FOR NURSING MANAGEMENT: A new tool that is more suitable for the Chinese hospital nursing context is available for evaluating Chinese clinical nurses' career success. Nursing managers can formulate appropriate management strategies according to the evaluation results to assist nurses in career development planning, thereby improving their career success level.

6.
ACS Appl Mater Interfaces ; 15(30): 36822-36830, 2023 Aug 02.
Artigo em Inglês | MEDLINE | ID: mdl-37467423

RESUMO

Despite the rapid development of versatile metal-organic frameworks (MOFs), the synthesis of water-stable MOFs remains challenging, which significantly limits their practical applications. Herein, a novel engineering strategy was developed to prepare superhydrophobic MOFs by an in situ fluorinated microporous organic network (FMON) coating. Through controllable modification, the resulting MOF@FMON retained the porosity and crystallinity of the pristine MOFs. Owing to the superhydrophobicity of the FMON and the feasibility of MOF synthesis, the FMON coating could be in situ integrated with various water-sensitive MOFs to provide superhydrophobicity. The coating thickness and hydrophobicity of the MOF@FMON composites were easily regulated by changing the FMON monomer concentration. The MOF@FMON composites exhibited excellent oil/water separation and catalytic activities and enhanced durability in aqueous solutions. This study provides a general approach for the synthesis of superhydrophobic MOFs, expanding the application scope of MOFs.

7.
Eur J Oncol Nurs ; 64: 102307, 2023 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-37141663

RESUMO

PURPOSE: Radiotherapy can negatively affect the pelvic floor function of patients with cervical cancer; however, the impact of different radiotherapy times and other related factors on pelvic floor function in cervical cancer survivors during radiotherapy remains unclear. We aimed to investigate the status of pelvic floor dysfunction (PFD) in cervical cancer survivors during radiotherapy and to analyze the factors influencing PFD. METHODS: In this cross-sectional study, a convenience sampling method was used to recruit cervical cancer survivors undergoing radiotherapy from January 2022 to July 2022 at a tertiary first-class hospital located in northeastern China. The Pelvic Floor Distress Inventory-Short Form 20 was used for participants' self-report of their PFD during radiotherapy. RESULTS: Data from 120 cervical cancer survivors were included in this study. The results showed that the mean PFDI-20 total score was 32.69 ± 7.76. Multiple stepwise linear regression analysis showed that 56.9% of the variance in PFD was explained by age (ß = 0.25, p < 0.001), body mass index (ß = 0.32, p < 0.001), recurrence (ß = 0.29, p < 0.001), number of radiotherapy sessions (ß = 0.39, p < 0.001), and number of deliveries (ß = 0.35, p < 0.001). CONCLUSION: It is important to pay more attention to the PFD status of cervical cancer survivors receiving radiotherapy. Future therapeutic approaches should involve early identification of relevant risk factors early to provide patients with personalized care at different stages of radiotherapy for reducing their discomfort and improving their health-related quality of life.


Assuntos
Sobreviventes de Câncer , Distúrbios do Assoalho Pélvico , Neoplasias do Colo do Útero , Feminino , Humanos , Distúrbios do Assoalho Pélvico/etiologia , Neoplasias do Colo do Útero/radioterapia , Estudos Transversais , Diafragma da Pelve , Qualidade de Vida , Inquéritos e Questionários
8.
Anal Bioanal Chem ; 415(18): 4533-4543, 2023 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-37017725

RESUMO

Recently, the good physical and chemical properties, well-defined pore architectures, and designable topologies have made microporous organic networks (MONs) excellent potential candidates in high-performance liquid chromatography (HPLC). However, their superior hydrophobic structures restrict their application in the reversed-phase mode. To solve this obstacle and to expand the application of MONs in HPLC, we realized the thiol-yne "click" postsynthesis of a novel hydrophilic MON-2COOH@SiO2-MER (MER denotes mercaptosuccinic acid) microsphere for reversed-phase/hydrophilic interaction mixed-mode chromatography. SiO2 was initially decorated with MON-2COOH using 2,5-dibromoterephthalic acid and tetrakis(4-ethynylphenyl)methane as monomers, and MER was then grafted via thiol-yne click reaction to yield MON-2COOH@SiO2-MER microspheres (5 µm) with a pore size of ~1.3 nm. The -COOH groups in 2,5-dibromoterephthalic acid and the post-modified MER molecules considerably improved the hydrophilicity of pristine MON and enhanced the hydrophilic interactions between the stationary phase and analytes. The retention mechanisms of the MON-2COOH@SiO2-MER packed column were fully discussed with diverse hydrophobic and hydrophilic probes. Benefiting from the numerous -COOH recognition sites and benzene rings within MON-2COOH@SiO2-MER, the packed column exhibited good resolution for the separation of sulfonamides, deoxynucleosides, alkaloids, and endocrine-disrupting chemicals. A column efficiency of 27,556 plates per meter was obtained for the separation of gastrodin. The separation performance of the MON-2COOH@SiO2-MER packed column was also demonstrated by comparing with those of MON-2COOH@SiO2, commercial C18, ZIC-HILIC, and bare SiO2 columns. This work highlights the good potential of the thiol-yne click postsynthesis strategy to construct MON-based stationary phases for mixed-mode chromatography.


Assuntos
Alcaloides , Dióxido de Silício , Dióxido de Silício/química , Cromatografia Líquida de Alta Pressão/métodos , Alcaloides/análise , Interações Hidrofóbicas e Hidrofílicas , Compostos de Sulfidrila , Cromatografia de Fase Reversa/métodos
9.
Talanta ; 257: 124391, 2023 May 15.
Artigo em Inglês | MEDLINE | ID: mdl-36854206

RESUMO

Microporous organic networks (MONs) are promising materials for the magnetic solid-phase extraction (MSPE) of trace targets from diverse complex samples. However, all the reported magnetic MONs (MMONs) are mono-functionalized and synthesized by refluxing at high temperatures, which is not an energy-efficient and environmentally friendly method. Here, for the first time, we report the room-temperature fabrication of a novel dual-functionalized MMON (MMON-B) for the efficient MSPE of typical vanillin additives from food samples prior to high-performance liquid chromatography (HPLC). The conjugated MMON-B with numerous -OH and -NH2 groups afforded good extraction for vanillins via π-π, hydrophobic, and hydrogen-bonding interactions. The factors affecting the extraction were studied in detail. Under the optimal conditions, the developed MMON-B-MSPE-HPLC-UV method exhibited wide linear range (0.50-1200 µg L-1), low limits of detection (0.10-0.15 µg L-1), and good reusability and stability. Therefore, MMON-B was successfully used to enrich vanillins in complex food samples. The morphology and extraction efficiency of the room-temperature synthesized MMON-B were comparable with those of the MMON-B synthesized via the conventional reflux method, indicating that the room-temperature fabrication method is a good alternative to the reflux method. This study presents the feasibility of using a room-temperature method for synthesizing dual-functionalized MONs, and the findings may significantly promote the application of MONs in the MSPE of trace targets from complex matrices.


Assuntos
Alimentos , Magnetismo , Temperatura , Fenômenos Magnéticos , Extração em Fase Sólida/métodos , Cromatografia Líquida de Alta Pressão , Limite de Detecção
10.
J Hazard Mater ; 443(Pt B): 130268, 2023 02 05.
Artigo em Inglês | MEDLINE | ID: mdl-36327830

RESUMO

Microporous organic networks (MONs) are a booming class of functional materials in elimination of environmental pollutants. However, the limit varieties of MONs still restrict their broad applications. Here we report the synthesis of a novel type of crown ether (CE)-based MONs via the coupling between brominated 18-crown-6 ether and different aromatic alkynyls. The constructed CE-based MONs integrates the good conjugation property of MONs and the inherent host-guest binding sites of CE, allowing the ultrafast and efficient adsorption and removal of a typical environmental priority pollutant 2,4,6-trichlorophenol (2,4,6-TCP). The hydrophobic CE-based MONs can also address the recovery challenge of unstable discrete CE in most organic and inorganic solvents. All CE-based MONs displayed fast adsorption kinetics (< 3 min) and large adsorption capacities (229.1-341.7 mg g-1) for 2,4,6-TCP. The CE-based MONs also gave stable adsorption capacities for 2,4,6-TCP in pH range of 4.0-6.0, NaCl concentration of 0-40 mg L-1, HA concentration of 0-30 mg L-1, or H2O2 ratio of < 5 %. Density functional theory calculation, Fourier transform infrared and X-ray photoelectron spectra evaluation revealed adsorption process involved hydrophobic, π-π and hydrogen bonding interactions. The CE-based MONs also showed favorable reusability and good adsorption for other toxic chlorophenols. This work highlights the potential of CE-based MONs in contaminants elimination.


Assuntos
Clorofenóis , Éteres de Coroa , Poluentes Ambientais , Poluentes Químicos da Água , Clorofenóis/química , Peróxido de Hidrogênio , Adsorção , Poluentes Ambientais/química , Poluentes Químicos da Água/análise
11.
Talanta ; 251: 123763, 2023 Jan 01.
Artigo em Inglês | MEDLINE | ID: mdl-35932636

RESUMO

Microporous organic networks (MONs) are promising in high performance liquid chromatography (HPLC) with large specific surface area, good hydrophobicity and stability. However, their superhydrophobic structures restrict MONs-based HPLC only in reversed-phase mode. To decrease the hydrophobicity of pristine MONs and to expand their broad application in HPLC, here we described the monomer-mediated fabrication of core-shell MON-2COOH@SiO2 microspheres for reversed-phase liquid chromatography (RPLC)/hydrophilic interaction liquid chromatography (HILIC) mixed-mode chromatography for the first time. The -COOH groups were introduced into MONs' skeleton to improve their hydrophilicity and to provide hydrophilic interaction sites. The MON-2COOH was grafted onto silica via a monomer mediated method to produce monodispersed core-shell microspheres. By adjusting the concentration of reactants, the thickness of MON-2COOH shell was easily manipulated. The packed MON-2COOH@SiO2 column showed high resolution and selectivity for separating both hydrophobic (alkylbenzenes, polycyclic aromatic hydrocarbons, anilines and phenols) and hydrophilic (nucleoside and nucleic bases) probes, highlighting the promise of MONs in mixed-mode HPLC. The MON-2COOH@SiO2 column also achieved good separation to sulfonamides, nonsteroidal anti-inflammatory drugs, flavonoids and phenylurea herbicides, and offered better resolution than commercial C18 and pristine SiO2 column. Multiple retention mechanisms were also found on MON-2COOH@SiO2 packed column, underlining the great potential of MONs in mixed-mode HPLC.


Assuntos
Herbicidas , Hidrocarbonetos Policíclicos Aromáticos , Compostos de Anilina , Anti-Inflamatórios , Cromatografia de Fase Reversa/métodos , Flavonoides , Interações Hidrofóbicas e Hidrofílicas , Microesferas , Nucleosídeos , Fenóis , Dióxido de Silício/química , Sulfonamidas
12.
J Hazard Mater ; 424(Pt B): 127485, 2022 02 15.
Artigo em Inglês | MEDLINE | ID: mdl-34655878

RESUMO

Microporous organic networks (MONs) have shown great potential in the removal of environmental contaminants. However, all studies have focused on the design and construction of novel and efficient adsorbents, and the recycling and reuse of adsorbates were disregarded. In this study, we report a feasible approach to synthesize renewable and reusable MONs by using target halogenated contaminants such as tetrabromobisphenol A (TBBPA), 2,3-dichlorophenol (2,3-DCP), and 2,4,6-trichlorophenol (2,4,6-TCP) as starting monomers. TBBPA, 2,3-DCP, and 2,4,6-TCP acted as hazardous contaminants and starting monomers for MONs, leading to the recycling of both adsorbents and adsorbates. The obtained TBBPA-MON, 2,3-DCP-MON, and 2,4,6-TCP-MON not only offered good reusability and large adsorption capacity for their elimination but also provided good adsorption for other phenolic contaminants relying on multiple interactions. Density functional theory calculation indicated the dominant role of π-π and hydrophobic interactions and the secondary role of hydrogen bonding interactions during the adsorption process. The used TBBPA-MON could be reused and the eluted TBBPA could be recycled and renewed for the construction of fresh MONs. This study provided a feasible approach to design and synthesize renewable MONs for environmental contaminants.


Assuntos
Fenóis , Adsorção , Ligação de Hidrogênio , Interações Hidrofóbicas e Hidrofílicas
13.
J Geriatr Cardiol ; 18(8): 623-630, 2021 Aug 28.
Artigo em Inglês | MEDLINE | ID: mdl-34527028

RESUMO

OBJECTIVE: To compare the morphological and compositional characteristics of carotid plaques in two cohorts (2002-2005 and 2012-2015) of Chinese patients using magnetic resonance vessel wall imaging. METHODS: Symptomatic patients with carotid atherosclerotic plaques who underwent carotid vessel wall magnetic resonance imaging between 2002-2005 and 2012-2015 were retrospectively recruited. Plaque morphology [including mean wall area, wall thickness, and maximum normalized wall index (NWI)] and composition [including calcification, intraplaque hemorrhage, and lipid-rich necrotic core (LRNC)] in symptomatic carotid arteries were evaluated and compared between patients in these two time periods. RESULTS: A total of 258 patients, including 129 patients in the 2002-2005 cohort and 129 patients in the 2012-2015 cohort, were recruited. Statin use (49.6%vs. 32.6%, P = 0.004) and hypertension (76.0% vs. 62.8%, P = 0.015) were significantly more common in the 2012-2015 cohort than in the 2002-2005 cohort. Patients in the 2012-2015 cohort also exhibited significantly low plaque burden parameters (allP < 0.05), as well as a lower prevalence (68.2% vs. 89.9%, P < 0.001) and volume percentages of LRNC (11.2% ± 14.2% vs. 25.7% ± 17.7%, P < 0.001). These differences remained significant after adjustment for clinical factors. The differences in the volume percentages of LRNC also remained significant after an additional adjustment for maximum NWI ( P < 0.001). CONCLUSIONS: Patients in the 2012-2015 cohort had a lower plaque burden and volume percentages of LRNC in symptomatic carotid arteries than those in the 2002-2005 cohort. These findings indicate that carotid plaques in the recent cohort had a lower severity and vulnerability.

14.
J Chromatogr A ; 1655: 462521, 2021 Oct 11.
Artigo em Inglês | MEDLINE | ID: mdl-34509692

RESUMO

As an effective sample pretreatment approach, stir bar sorptive extraction (SBSE) has shown great prospects in static microextraction and selective enrichment. In this work, bifunctional microporous organic network (B-MON) with the coexistence of amino and hydroxyl groups was firstly designed and synthesized as a novel coating for efficient SBSE of parabens and flavors in combination with high-performance liquid chromatography coupled with photodiode array detection (HPLC-PDA). Linked by covalent bonds to form an extension of the aromatic ring skeleton, B-MON was a tailored adsorbent featured by porous structure and abundant hydrogen bonding sites for analytes with benzene/naphthalene rings and OH/COOH groups. The extraction and desorption parameters were evaluated in detail. Under the optimized conditions, the proposed B-MON-SBSE-HPLC-PDA method offered good linearity (0.10-100 µg L-1) with correlation coefficients R2 ≥ 0.995, low limits of detection (0.010-0.035 µg L-1) and limits of quantification (0.035-0.115 µg L-1), and favorable enrichment factors (40-49). Furthermore, the developed method has been applied to the analysis of parabens and flavors in cosmetic and food samples with recoveries ranging from 80.4 to 109.6%. This method was also feasible to extract the analytes with benzene/naphthalene rings and OH/COOH groups, such as the plant growth regulators and non-steroidal anti-inflammatory drugs. The present study provided a new way to synthesize bifunctional MONs for SBSE of trace analytes in complex samples.


Assuntos
Parabenos , Cromatografia Líquida de Alta Pressão , Limite de Detecção , Porosidade , Reprodutibilidade dos Testes
15.
ACS Appl Mater Interfaces ; 13(33): 39905-39914, 2021 Aug 25.
Artigo em Inglês | MEDLINE | ID: mdl-34374514

RESUMO

The lack of functional groups or binding sites largely hindered the broad application of microporous organic networks (MONs). Herein, we report the fabrication of the sulfonate group-enriched magnetic MON composite (MMON-SO3H@SO3Na) via the combination of the sulfonic acid group containing the monomer and thiol-yne click postmodification for efficient magnetic solid-phase extraction (MSPE) of benzimidazole fungicides (BZDs) from complex sample matrices. The well-defined core-shell-structured MMON-SO3H@SO3Na was obtained and served as an advanced adsorbent for MSPE for concentrating and monitoring trace BZDs. The MMON-SO3H@SO3Na with numerous sulfonate groups provides plenty of ion-exchange, hydrogen-bonding, and π-π sites, leading to the favorable affinity to BZDs via multiple interaction mechanisms. The MMON-SO3H@SO3Na-based MSPE-high-performance liquid chromatography method afforded a wide linear range, low limits of detection, large enrichment factors, good precisions, and reusability for BZDs. Trace BZDs in complex vegetables and fruit samples were successfully detected by the established method. The MMON-SO3H@SO3Na also exhibited good selectivity toward multiple types of polar contaminants containing hydrogen-bonding sites and aromatic structures. This work provided a new postsynthesis strategy for constructing novel and multifunctioned magnetic MONs for preconcentration of trace analytes in a complex matrix.


Assuntos
Alcanossulfonatos/síntese química , Alcinos/química , Benzimidazóis/isolamento & purificação , Análise de Alimentos/métodos , Fungicidas Industriais/isolamento & purificação , Compostos de Sulfidrila/química , Cromatografia Líquida de Alta Pressão/métodos , Química Click , Óxido Ferroso-Férrico/química , Frutas/química , Limite de Detecção , Magnetismo/métodos , Microesferas , Porosidade , Reprodutibilidade dos Testes , Extração em Fase Sólida/métodos , Verduras/química
16.
Talanta ; 233: 122471, 2021 Oct 01.
Artigo em Inglês | MEDLINE | ID: mdl-34215105

RESUMO

Development of novel functionalized adsorbents for efficient magnetic solid phase extraction (MSPE) is essential for promoting their versatile applications in sample pretreatment. Herein, we report the fabrication of a new polyethyleneimine-600 decorated magnetic microporous organic network nanosphere (Fe3O4@MON-PEI600) for effective MSPE of trace non-steroidal anti-inflammatory drugs (NSAIDs) from different water samples. The core-shelled Fe3O4@MON-PEI600 integrates the synergistic effects of Fe3O4, MON and PEI600, providing facile and effective extraction to NSAIDs via multiple hydrogen bonding, π-π and hydrophobic interactions. The inner MON shell employs π-π and hydrophobic interaction sites and the outer PEI-600 coat acts as the hydrogen bonding doner/receptor, which affords good extraction performance for NSAIDs. Under optimal conditions, the Fe3O4@MON-PEI600-MSPE-HPLC-UV method gives wide linear range (0.14-400 µg L-1), low limits of detection (0.042-0.149 µg L-1), good precisions (intra-day and inter-day RSDs < 4.5%, n = 6), and large enrichment factors (97.0-98.2). Extraction mechanisms and selectivity of Fe3O4@MON-PEI600 are evaluated in detail. Moreover, Fe3O4@MON-PEI600 is successfully applied to enrich the trace NSAIDs in different water samples with the concentrations of 0.7 and 0.8 µg L-1 for 1-naphthylacetic acid, 0.5 and 0.1 µg L-1 for naproxen as well as 0.7 µg L-1 for ibuprofen, respectively. The developed method not only affords a novel and efficient magnetic adsorbent for NSAIDs in aqueous media at trace level, but also provides a new strategy for the rational design and synthesis of multiple functionalized MON composites in sample pretreatment.


Assuntos
Nanosferas , Preparações Farmacêuticas , Adsorção , Anti-Inflamatórios não Esteroides , Cromatografia Líquida de Alta Pressão , Limite de Detecção , Fenômenos Magnéticos , Polietilenoimina , Extração em Fase Sólida , Águas Residuárias
17.
Electrophoresis ; 42(19): 1936-1944, 2021 10.
Artigo em Inglês | MEDLINE | ID: mdl-34180069

RESUMO

Microporous organic networks (MONs) that exhibit good stability and hydrophobicity are promising candidates for performing HPLC separation of small organic compounds. However, their applications in separating large analytes as well as biomolecules are still limited by the microporous nature of MONs. Herein, we demonstrated the fabrication of a MON-functionalized silica (MON@SiO2 ), exhibiting micro and mesopores for the HPLC separations of small drugs as well as large analytes, such as flavones, nonsteroidal anti-inflammatory drugs (NSAIDs), endocrine disrupting chemicals (EDCs), and proteins. MON was successfully modified on SiO2 microspheres to yield the uniform and mono-dispersed MON@SiO2 . The separation mechanisms and performance of the MON@SiO2 packed column were evaluated for a wide range of analytes, including neutral, acidic, basic compounds, drugs, and proteins. Compared with commercial C18 and SiO2 -NH2 packed columns, the proposed MON@SiO2 column afforded superior performance in the separations of flavones, NSAIDs, EDCs, and proteins. Moreover, the MON@SiO2 column also offered good repeatability with intraday RSDs (n = 7) of <0.1%, <2.0%, <2.3%, and <0.7% for the retention time, peak height, peak area, and half peak width, respectively, for separating EDCs. This work proved the potential of using MONs in the HPLC separations of drugs and proteins.


Assuntos
Disruptores Endócrinos , Flavonas , Preparações Farmacêuticas , Anti-Inflamatórios não Esteroides , Cromatografia Líquida de Alta Pressão , Proteínas , Dióxido de Silício
18.
J Chromatogr A ; 1651: 462347, 2021 Aug 16.
Artigo em Inglês | MEDLINE | ID: mdl-34166861

RESUMO

Herein, we report the fabrication of a novel, well-defined core-double-shell-structured magnetic Fe3O4@polydopamine@naphthyl microporous organic network (MON), Fe3O4@PDA@NMON, for the efficient magnetic extraction of hydroxylated polycyclic aromatic hydrocarbons (OH-PAHs) and p-nitrophenol (p-Npn) from wastewater samples. The hierarchical nanospheres were designed and constructed with the Fe3O4 nanoparticle core, the inner shell of a polydopamine (PDA) layer, and the outer shell of a porous naphthyl MON (NMON) coating, allowing efficient and synergistic extraction of OH-PAHs and p-Npn via hydrophobic, hydrogen bonding, and π-π interactions. The Fe3O4@PDA@NMON nanospheres were well characterized and employed as an efficient sorbent for magnetic solid-phase extraction (MSPE) coupled with high performance liquid chromatography (HPLC) for analyzing of OH-PAHs and p-Npn. Under optimal conditions, the Fe3O4@PDA@NMON-based-MSPE-HPLC-UV method afforded wide linear range (0.18-500 µg L-1), low limits of detection (0.070 µg L-1 for p-Npn, 0.090 µg L-1 for 2-OH-Nap, 0.090 µg L-1 for 9-OH-Fluo and 0.055 µg L-1 for 9-OH-Phe, respectively), large enrichment factors (92.6-98.4), good precisions (intra-day and inter-day relative standard deviations (RSDs); <6.4%, n=6) and less consumption of the adsorbent. Furthermore, trace OH-PAHs and p-Npn with concentrations of 0.29-0.80 µg L-1 were successfully detected in various wastewater samples. Fe3O4@PDA@NMON also functioned as a good adsorbent to enrich a wide scope of trace contaminants containing hydrogen bonding sites and aromatic structures, highlighting the potential of functional MONs in sample pretreatment.


Assuntos
Indóis/química , Nanosferas/química , Nitrofenóis/isolamento & purificação , Hidrocarbonetos Policíclicos Aromáticos/isolamento & purificação , Polímeros/química , Extração em Fase Sólida/métodos , Águas Residuárias/química , Cromatografia Líquida de Alta Pressão , Interações Hidrofóbicas e Hidrofílicas , Limite de Detecção , Fenômenos Magnéticos , Nitrofenóis/análise , Hidrocarbonetos Policíclicos Aromáticos/análise , Porosidade
19.
Front Oncol ; 11: 640738, 2021.
Artigo em Inglês | MEDLINE | ID: mdl-34055608

RESUMO

PURPOSE: To evaluate isocitrate dehydrogenase (IDH) status in clinically diagnosed grade II~IV glioma patients using the 2016 World Health Organization (WHO) classification based on MRI parameters. MATERIALS AND METHODS: One hundred and seventy-six patients with confirmed WHO grade II~IV glioma were retrospectively investigated as the study set, including lower-grade glioma (WHO grade II, n = 64; WHO grade III, n = 38) and glioblastoma (WHO grade IV, n = 74). The minimum apparent diffusion coefficient (ADCmin) in the tumor and the contralateral normal-appearing white matter (ADCn) and the rADC (ADCmin to ADCn ratio) were defined and calculated. Intraclass correlation coefficient (ICC) analysis was carried out to evaluate interobserver and intraobserver agreement for the ADC measurements. Interobserver agreement for the morphologic categories was evaluated by Cohen's kappa analysis. The nonparametric Kruskal-Wallis test was used to determine whether the ADC measurements and glioma subtypes were related. By univariable analysis, if the differences in a variable were significant (P<0.05) or an image feature had high consistency (ICC >0.8; κ >0.6), then it was chosen as a predictor variable. The performance of the area under the receiver operating characteristic curve (AUC) was evaluated using several machine learning models, including logistic regression, support vector machine, Naive Bayes and Ensemble. Five evaluation indicators were adopted to compare the models. The optimal model was developed as the final model to predict IDH status in 40 patients with glioma as the subsequent test set. DeLong analysis was used to compare significant differences in the AUCs. RESULTS: In the study set, six measured variables (rADC, age, enhancement, calcification, hemorrhage, and cystic change) were selected for the machine learning model. Logistic regression had better performance than other models. Two predictive models, model 1 (including all predictor variables) and model 2 (excluding calcification), correctly classified IDH status with an AUC of 0.897 and 0.890, respectively. The test set performed equally well in prediction, indicating the effectiveness of the trained classifier. The subgroup analysis revealed that the model predicted IDH status of LGG and GBM with accuracy of 84.3% (AUC = 0.873) and 85.1% (AUC = 0.862) in the study set, and with the accuracy of 70.0% (AUC = 0.762) and 70.0% (AUC = 0.833) in the test set, respectively. CONCLUSION: Through the use of machine-learning algorithms, the accurate prediction of IDH-mutant versus IDH-wildtype was achieved for adult diffuse gliomas via noninvasive MR imaging characteristics, including ADC values and tumor morphologic features, which are considered widely available in most clinical workstations.

20.
Turk Neurosurg ; 31(6): 880-887, 2021.
Artigo em Inglês | MEDLINE | ID: mdl-33759171

RESUMO

AIM: To analyze certain magnetic resonance imaging (MRI) features as well as six major genetic biomarkers, investigated their associations, and evaluated their prognostic roles in glioblastomas (GBMs). MATERIAL AND METHODS: Strict criteria included newly diagnosed GBM with optimal treatments. Simple manual imaging characteristics (tumor side, location, enhancement, diameter, depth, radiographic necrosis, and edema) were obtained from preoperative conventional MRI. Furthermore, all the status of the MGMT promoter, Chromosome 1p and 19q, IDH, TERT, and BRAF in tumor tissues were detected. RESULTS: Among 126 inpatients, 60 cases were selected and enrolled in the study. The status of the MGMT promoter was significantly associated with the grade of radiographic necrosis (p=0.033). The rate of 19q deletion was significantly higher in tumors with the ring-shaped peritumoral edema (PTE) (p=0.035) and in tumors with the ring-enhanced trait (p=0.023). Univariate analysis showed that a low PTE index and MGMT promoter methylation were both unfavorable prognostic factors. While the PTE index statistically dropped out, the status of the MGMT promoter and the depth of the tumor were observed to be independent prognostic factors in multivariate analysis. CONCLUSION: Based on simple neuroimaging metrics, novel connections between features of preoperative conventional MRI and status of major genetic biomarkers were observed, especially for the MGMT promoter and 19q.


Assuntos
Neoplasias Encefálicas , Glioblastoma , Biomarcadores , Biomarcadores Tumorais/genética , Neoplasias Encefálicas/diagnóstico por imagem , Neoplasias Encefálicas/genética , Metilação de DNA , Metilases de Modificação do DNA/genética , Enzimas Reparadoras do DNA/genética , Glioblastoma/genética , Humanos , Imageamento por Ressonância Magnética , Prognóstico , Proteínas Supressoras de Tumor/genética
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