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1.
Anal Chem ; 2024 Sep 13.
Artigo em Inglês | MEDLINE | ID: mdl-39269845

RESUMO

The sensitive detection of trace biomarkers in exhaled breath for lung cancer diagnosis represents a critical area of research in life analytical chemistry, with profound implications for early disease detection, therapeutic intervention, and prognosis monitoring. Despite its potential, the analytical process faces significant challenges due to the ultratrace levels of disease biomarkers present and the complex, high-humidity composition of exhaled breath. This study introduces a highly sensitive method for detecting aldehyde biomarkers in exhaled breath by integrating the use of amino-functionalized microporous organic networks (NH2-MON) as a solid-phase microextraction (SPME) fiber coating with gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) analysis. The method innovatively combines sample collection and extraction, achieving a dual-step enrichment process that significantly enhances both the enrichment efficiency and reproducibility of biomarker detection while effectively mitigating the interference caused by water vapor in exhaled breath. The NH2-MON, utilized as an SPME fiber coating, demonstrates exceptional enrichment capacity for five key aldehyde biomarkers, facilitating the development of a highly sensitive detection approach for these biomarkers in exhaled breath. Compared to previously reported methods, the proposed technique exhibits significantly lower limits of quantification, ranging from 0.77 to 11.89 pg mL-1, and achieves substantially higher enrichment factors, ranging from 9156- to 35723-fold. The practicality and feasibility of the method were validated through the analysis of exhaled breath samples from lung cancer patients, underscoring its potential application in the early diagnosis and monitoring of lung cancer.

2.
Food Res Int ; 192: 114833, 2024 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-39147522

RESUMO

This study examined the suppressive effects of 16 selected plant-based foods on α-glucosidase and pancreatic lipase and their antioxidant properties. Among these, the bark of Cinnamomum cassia (Cinnamon, WLN-FM 15) showed the highest inhibitory activity against α-glucosidase and the highest antioxidant activity. Additionally, WLN-FM 15 showed promising results in the other tests. To further identify the bioactive constituents of WLN-FM 15, a multi-bioactivity-labeled molecular networking approach was used through a combination of GNPS-based molecular networking, DPPH-HPLC, and affinity-based ultrafiltration-HPLC. A total of nine procyanidins were identified as antioxidants and inhibitors of α-glucosidase and pancreatic lipase in WLN-FM 15. Subsequently, procyanidins A1, A2, B1, and C1 were isolated, and their efficacy was confirmed through functional assays. In summary, WLN-FM 15 has the potential to serve as a functional food ingredient with the procyanidins as its bioactive constituents. These results also suggest that the multi-bioactivity-labeled molecular networking approach is reliable for identifying bioactive constituents in plant-based foods.


Assuntos
Antioxidantes , Biflavonoides , Catequina , Cinnamomum aromaticum , Inibidores de Glicosídeo Hidrolases , Lipase , Casca de Planta , Proantocianidinas , Proantocianidinas/farmacologia , Proantocianidinas/química , Proantocianidinas/análise , Lipase/antagonistas & inibidores , Lipase/metabolismo , Antioxidantes/farmacologia , Antioxidantes/química , Antioxidantes/análise , Inibidores de Glicosídeo Hidrolases/farmacologia , Inibidores de Glicosídeo Hidrolases/química , Casca de Planta/química , Cinnamomum aromaticum/química , Biflavonoides/farmacologia , Biflavonoides/análise , Biflavonoides/química , Catequina/análise , Catequina/química , Catequina/farmacologia , Extratos Vegetais/química , Extratos Vegetais/farmacologia , Cromatografia Líquida de Alta Pressão , Pâncreas/enzimologia , alfa-Glucosidases/metabolismo , Farmacologia em Rede , Inibidores Enzimáticos/farmacologia , Inibidores Enzimáticos/química
3.
J Agric Food Chem ; 72(22): 12822-12831, 2024 Jun 05.
Artigo em Inglês | MEDLINE | ID: mdl-38803050

RESUMO

The identification of dietary exposure biomarkers is crucial for advancing our understanding of the health benefits of specific foods. Broccoli, a vegetable with well-known anticancer properties, contains active ingredients, such as isothiocyanates with indole side chains. Hence, indole metabolites related to broccoli consumption have the potential to serve as biomarkers of dietary exposure. In this work, we developed a new analytical method for indole metabolites in urine using a poly(deep eutectic solvents)-molecularly imprinted polymer/vinyl-functionalized graphene oxide (PDESs-MIP/VGO) in miniaturized centrifugal pipet-tip solid-phase extraction (CPT-SPE) coupled with liquid chromatography. This method integrates the strengths of PDESs-MIP/VGO, including rich adsorption interactions, high adsorption capacity, and excellent selectivity, with the simplicity and cost-effectiveness of CPT-SPE. The proposed method demonstrated low limits of quantification (1.2-2.5 ng mL-1), high accuracy (91.7-104.8%), and good precision (relative standard deviation ≤4.4%). By applying this method to analyze indole metabolites in urine, our results suggested that indole-3-carbinol and indole-3-acetonitrile have the potential to emerge as reliable dietary exposure biomarkers for broccoli intake. Furthermore, highly selective analytical methods based on molecular imprinting technology are advantageous for precise screening and analysis of dietary exposure biomarkers associated with food consumption.


Assuntos
Biomarcadores , Brassica , Indóis , Extração em Fase Sólida , Humanos , Indóis/urina , Indóis/metabolismo , Biomarcadores/urina , Brassica/química , Brassica/metabolismo , Extração em Fase Sólida/métodos , Exposição Dietética , Cromatografia Líquida de Alta Pressão/métodos , Polímeros Molecularmente Impressos/química , Polímeros Molecularmente Impressos/metabolismo , Grafite
4.
Chem Sci ; 15(16): 6002-6011, 2024 Apr 24.
Artigo em Inglês | MEDLINE | ID: mdl-38665520

RESUMO

Nanozymes have gained much attention as a replacement for natural enzymes duo to their unique advantages. Two-dimensional layered double hydroxide (LDH) nanomaterials with high physicochemical plasticity are emerging as the main forces for the construction of nanozymes. Unfortunately, high-performance LDH nanozymes are still scarce. Recently, defects in nanomaterials have been verified to play a significant role in modulating the catalytic microenvironment, thereby improving catalytic performances of nanozymes. Therefore, the marriage between defect engineering and LDH nanozymes is expected to spark new possibilities. In this work, twenty kinds of natural amino acids were separately inserted into the interlayer of CoFe-LDH to obtain defect-rich CoFe-LDH nanozymes. The peroxidase (POD)-like activity and catalytic mechanism of the as-prepared LDH nanozymes were systematically studied. The results showed that the intercalation of amino acids can effectively enhance the POD-like activity of LDH nanozymes owing to the increasing oxygen/metal vacancies. And l-cysteine intercalated LDH exhibited the highest catalytic activity ascribed to its thiol group. As a proof of concept, LDH nanozymes with superb POD-like activity were used in biosensing and antibacterial applications. This work suggests that modulating the catalytic microenvironment through defect engineering is an effective way to obtain high-efficiency POD mimics.

5.
Anal Chim Acta ; 1294: 342289, 2024 Mar 15.
Artigo em Inglês | MEDLINE | ID: mdl-38336412

RESUMO

BACKGROUND: The detection of disease biomarkers in biological samples plays an important role in early diagnosis and treatment of carcinoid tumor. However, due to the complexity of biological samples and the extremely low concentration of disease biomarkers, sample pretreatment is still the bottleneck of achieving accurate quantitative determination. In this work, new hydrophilic molecularly imprinted resin-hexagonal boron nitride (HMIR-h-BN) composites were developed and used as a new solid phase extraction (SPE) adsorbent for selective detection of 5-hydroxyindoleacetic acid (5-HIAA), a biomarker of carcinoid tumor, in urine. RESULTS: Twenty-two types of HMIR-h-BN were successfully synthesized through growing hydrophilic molecularly imprinted resin on surface of activated two-dimensional h-BN nanosheets, and preparation parameters affecting the adsorption performance of HMIR-h-BN were investigated and optimized through adsorption experiments. HMIR-h-BN #19 (the ratio of resorcinol to hexamethylenetetramine: 6:3; the dosage of h-BN: 300 mg; the dosage of dummy template: 0.12 mmol; the imprinting time: 4 h) has demonstrated to be the optimal material for efficient separation and extraction of 5-HIAA. Combined with HPLC-UV, the limit of detection and the limit of quantification of 5-HIAA in real urine samples were 9.4 ng mL-1 and 31.3 ng mL-1, respectively, the coefficient of determination (R2) was 0.9996 in the linear range of 0.1-300 µg mL-1 and the relative recoveries ranged from 86.9 % to 97.7 % with RSD ≤5.1 %. Moreover, after being processed by HMIR-h-BN-SPE, there are no interferences from other peaks at the peak position of 5-HIAA. SIGNIFICANCE: The HMIR-h-BN composite has been demonstrated to be capable of selective extraction of 5-HIAA from urine samples and have a significant purification effect. Based on the established HMIR-h-BN-SPE-HPLC-UV method, accurate quantitative determination of 5-HIAA in urine samples was achieved, which is expected to be applied in the early diagnostic of carcinoid tumor.


Assuntos
Compostos de Boro , Tumor Carcinoide , Impressão Molecular , Humanos , Biomarcadores Tumorais , Ácido Hidroxi-Indolacético , Extração em Fase Sólida/métodos , Impressão Molecular/métodos , Cromatografia Líquida de Alta Pressão , Adsorção
6.
J Chromatogr A ; 1715: 464599, 2024 Jan 25.
Artigo em Inglês | MEDLINE | ID: mdl-38150874

RESUMO

Overweight and obesity are the causes of many diseases and have become global "epidemics". Research on natural active components with anti-adipogenesis effects in plants has aroused the interest of researchers. One of the most critical problems is establishing sample preparation and analytical techniques for quickly and selectively extracting and determining the active anti-adipogenesis components in complex plant matrices for developing new anti-adipogenic drugs. In this study, a new poly(deep eutectic solvents) surface imprinted graphene oxide composite (PDESs-MIP/GO) with high selectivity for phenolic acids was prepared using deep eutectic solvents as monomers and crosslinkers. A miniaturized centrifugation-accelerated pipette-tip matrix solid-phase dispersion method (CPT-MSPD) with PDESs-MIP/GO as adsorbent, coupled with high-performance liquid chromatography, was further developed for the rapid determination of anti-adipogenesis markers in Solidago decurrens Lour. (SDL). The established method was successfully used to determination anti-adipogenesis markers in SDL from different regions, with the advantages of accuracy (recoveries: 94.4 - 115.9 %, RSDs ≤ 9.8 %), speed (CPT-MSPD time: 11 min), selectivity (imprinting factor: ∼2.0), and economy (2 mg of adsorbent and 1 mL of solvents), which is in line with the current advanced principle of "3S+2A" in analytical chemistry.


Assuntos
Solventes Eutéticos Profundos , Grafite , Solidago , Extração em Fase Sólida/métodos , Solventes/química , Cromatografia Líquida de Alta Pressão
7.
J Chromatogr A ; 1714: 464578, 2024 Jan 11.
Artigo em Inglês | MEDLINE | ID: mdl-38104506

RESUMO

Alectinib is known as an effective targeted drug, which has excellent therapeutic effect on non-small cell lung cancer and can significantly prolong the survival of patients. Therapeutic drug monitoring is necessary due to the photo-instability of alectinib and the individual differences in patients. In this work, a porous polydopamine graphene oxide composite (PDAG) was prepared by a simple surface modification method. A PDAG-based pipette-tip solid-phase extraction (PT-SPE) coupled with HPLC-UV detection was proposed for the separation and detection of alectinib and its active metabolite M4 in plasma. The method was methodologically validated and showed good linearity in the range of 50-5000 ng mL-1 (R2 > 0.9995). The limit of detection (LOD) was 4.8 ng mL-1 and 3.9 ng mL-1 for alectinib and M4, respectively, and the limit of quantitation (LOQ) was 16.1 ng mL-1 and 13.1 ng mL-1, respectively. The intra-day and inter-day precision expressed by coefficient of variation was less than 4.8 %. The recovery of this method ranged from 84.9 % to 103.5 % with a standard deviation of less than 4.3 %. In conclusion, the established method is accurate, stable and inexpensive, and can be used to monitor the levels of alectinib and M4 in plasma, which provide technical and data support for exploring optimal individualized remedial dosing regimens.


Assuntos
Carcinoma Pulmonar de Células não Pequenas , Neoplasias Pulmonares , Humanos , Cromatografia Líquida de Alta Pressão/métodos , Porosidade , Carcinoma Pulmonar de Células não Pequenas/tratamento farmacológico , Extração em Fase Sólida/métodos
8.
J Chromatogr A ; 1711: 464448, 2023 Nov 22.
Artigo em Inglês | MEDLINE | ID: mdl-37852047

RESUMO

Simultaneous determination of multiple biomarkers can improve the effectiveness and accuracy of cancer diagnosis. Cortisol, cortisone, and 4-methoxyphenylacetic acid (4-Me) are metabolic biomarker group with high specificity and sensitivity for the diagnosis of non-small cells lung cancer (NSCLC), and the development of their simultaneous determination method is desired. Herein, a simple, sensitive, and low-cost method involving pipette-tip solid-phase extraction (PT-SPE) using anion exchange adsorbent (MAX) coupled with liquid chromatography tandem mass spectrometry (LC-MS/MS) was developed for the simultaneous determination of three biomarkers (cortisol, cortisone, and 4-Me) in human urine. The sample (0.1 mL), adsorbent (1.5 mg) and organic reagent (3.5 mL) of MAX-PT-SPE are less consumed, and have the advantages of easy access to raw materials, simple assembly, convenient on-site instant extraction, low pollution, and low cost. The limits of detection of the three biomarkers were 0.006-0.024 ng mL-1, the recoveries of three spiked levels (2, 50, and 500 ng mL-1) were 91.0%-99.3%, with the relative standard deviations (RSDs) ≤ 5.9%. Finally, the MAX-PT-SPE-LC-MS/MS method achieved the quantitative analysis of cortisol, cortisone, and 4-Me in urine of different patients of NSCLC. This method is expected to be used in the non-invasive auxiliary diagnosis of NSCLC, and it provides a new strategy for multi-molecular diagnosis and multi-omics combined diagnosis.


Assuntos
Cortisona , Neoplasias Pulmonares , Humanos , Cromatografia Líquida , Espectrometria de Massas em Tandem , Hidrocortisona , Neoplasias Pulmonares/diagnóstico , Extração em Fase Sólida/métodos , Cromatografia Líquida de Alta Pressão/métodos
9.
J Chromatogr A ; 1705: 464224, 2023 Aug 30.
Artigo em Inglês | MEDLINE | ID: mdl-37490816

RESUMO

Osimertinib (OSIM) is widely used as a mainstream drug for the treatment of non-small cell lung cancer (NSCLC). However, the lack of a rapid extraction and detection method for OSIM and its metabolite, AZ-5104, has limited clinical drug metabolism and drug resistance research because the drug is unstable. In this study, a new ionic liquid hybrid hierarchical porous material (IL-HHPM) was synthesized with hierarchical porous structures, including micropores (1.6-2.0 nm), mesopores (2.0-50.0 nm), macropores (50.0-148.7 nm), and multiple functional groups via a one-step hydrothermal method using silanized ionic liquids (IL) as functionalized hybrid monomer. The IL-HHPM has the advantages of a high specific surface area (437.4 ± 4.6 m2 g-1), sizable pore volume (0.74 cm3 g-1), and fast mass transfer, additionally, the IL-HHPM adsorbed OSIM and AZ-5104 via π-π interactions and hydrogen bonding. OSIM and AZ-5104 were rapidly extracted and measured in human urine using rapid and miniaturized centrifugal spin-column extraction (MCSCE), which was based on the IL-HHPM. The optimized factors for the extraction recoveries of OSIM and AZ-5104 were adsorbent dosage (8.0 mg), sample volume (0.5 mL), and operation time (9.0 min), and markedly reduced the adsorbent dosage and operation time. The IL-HHPM-MCSCE-HPLC method displayed good linearity (0.02-5.00 µg mL-1, r ≥ 0.9997), satisfying accuracy (spiked recoveries of 87.7%-100.0%), and good precision (RSDs ≤ 7.0%). The developed method is rapid, sensitive, and reproducible for the simultaneous determination of trace level of OSIM and AZ-5104 in human urine.


Assuntos
Carcinoma Pulmonar de Células não Pequenas , Líquidos Iônicos , Neoplasias Pulmonares , Humanos , Líquidos Iônicos/química , Porosidade , Cromatografia Líquida de Alta Pressão/métodos , Extração em Fase Sólida/métodos
10.
J Chromatogr A ; 1690: 463787, 2023 Feb 08.
Artigo em Inglês | MEDLINE | ID: mdl-36652815

RESUMO

Alectinib and its metabolite, M4, have demonstrated a satisfactory clinical therapeutic effect in the treatment of anaplastic lymphoma kinase-positive advanced non-small-cell lung cancer. Due to individual differences among patients, therapeutic drug monitoring (TDM) is critical for guaranteeing appropriate clinical drug use. To realize TDM for alectinib and its metabolite, M4, a honeycomb phenol-formaldehyde resin (PFR) with excellent hydrophilic properties, abundant adsorption force, and a stable porous structure was synthesized by modifying the porogens F127 and P123. The prepared PFR was employed as an adsorbent in a simple and efficient spin-column solid-phase extraction (SPE) process. A rapid method for detecting alectinib and its metabolite M4 in urine was thereby established. The established method showed a linear range of 0.0200 µg mL-1-5.00 µg mL-1 and the recovery range of 98.8-103% for spiked urine samples, with relative standard deviations of ≤ 4.87% (n = 3). Our results proved the practicability of the proposed honeycomb-PFR spin-column SPE method in TDM for alectinib and its metabolite, M4.


Assuntos
Carcinoma Pulmonar de Células não Pequenas , Neoplasias Pulmonares , Humanos , Carcinoma Pulmonar de Células não Pequenas/tratamento farmacológico , Neoplasias Pulmonares/tratamento farmacológico , Piperidinas , Extração em Fase Sólida
11.
Diabetes Obes Metab ; 25(2): 342-353, 2023 02.
Artigo em Inglês | MEDLINE | ID: mdl-36200449

RESUMO

Gestational diabetes mellitus (GDM) is a common complication of pregnancy, affecting 14% of pregnancies worldwide, and the prevention of pathological hyperglycaemia during pregnancy is meaningful for global public health. The role of iron supplementation in the progression of GDM has been of significant interest in recent years. Iron is a micronutrient that is vital during pregnancy; however, given the toxic properties of excess iron, it is probable that prophylactic iron supplementation will increase the risk of adverse pregnancy outcomes, including GDM. It is critical to clarify the effect of iron supplementation on the risk of GDM. Therefore, in this review, we comprehensively assess the role of iron in pregnancy. This review aimed to analyse the necessity of iron supplementation and maintenance of iron homeostasis during pregnancy, particularly reviewing the role and function of iron in beta cells and examining the mechanisms of excess iron contributing to the pathogenesis of GDM. Moreover, we aimed to discuss the association of haemoglobin and ferritin with GDM and identify priority areas for research.


Assuntos
Diabetes Gestacional , Gravidez , Feminino , Humanos , Diabetes Gestacional/prevenção & controle , Ferro/efeitos adversos , Ferritinas , Resultado da Gravidez , Suplementos Nutricionais/efeitos adversos
12.
Food Chem ; 398: 133920, 2023 Jan 01.
Artigo em Inglês | MEDLINE | ID: mdl-35988418

RESUMO

The overuse of swelling agents in fruits and vegetables has rapidly increased, resulting in food safety problems. Hence, a new method for the selective extraction and detection of thidiazuron (TDZ) and forchlorfenuron (KT30) was developed using deep eutectic solvent-molecularly imprinted hydrophilic resin (DES-MIHR) as a pipette tip solid-phase extraction (PT-SPE) adsorbent with excellent molecular recognition in aqueous matrixes. DES-MIHR interacted with TDZ and KT30 via π-π interactions and hydrogen bonding. The miniaturized PT-SPE can be performed with just 5.0 mg adsorbent, 0.3 mL water, and 0.2 mL eluent, thus having the advantage of the low consumption of adsorbent and organic reagents. The performance of the DES-MIHR-PT-SPE-high-performance liquid chromatography (HPLC) method was demonstrated with the recoveries from various fruits and vegetables being 81.1-102.9 % (RSD ≤ 7.1 %). Thereby indicating the general applicability of the developed method for the accurate determination of trace swelling agents in fruits and vegetables.


Assuntos
Impressão Molecular , Verduras , Cromatografia Líquida de Alta Pressão , Solventes Eutéticos Profundos , Frutas , Impressão Molecular/métodos , Extração em Fase Sólida/métodos
13.
J Chromatogr A ; 1677: 463288, 2022 Aug 16.
Artigo em Inglês | MEDLINE | ID: mdl-35820230

RESUMO

In this study, a new rapid and inexpensive filter solid-phase extraction method (FSPE) was developed for the extraction and separation of five perfluorinated carboxylic acids (PFCAs) (namely, perfluorooctanoic acid, perfluorononanoic acid, perfluorodecanoic acid, perfluoroundecanoic acid, and perfluorododecanic acid) from milk samples. Commercial nylon 66 syringe filters were used as adsorbents without additional modification. The proposed method could achieve the fast adsorption of analytes by benefitting from the advantages of using the nylon 66 filter membrane on PFCAs with multiple adsorption interactions, namely, hydrophobic interactions and hydrogen bonds. The FSPE was designed to achieve the rapid isolation of analytes based on the rapid solid-liquid separation while using the solid-phase extraction disk. PFCAs residues in milk were extracted by first flowing the samples through a nylon 66 syringe filter from top to bottom. Double contact desorption with methanol was then accomplished by pulling and pushing the syringe, followed by derivatization with acetyl chloride-methanol. Finally, the extracted PFCAs residues were monitored using gas chromatography-tandem mass spectrometry (GC-MS/MS) quantification. Under optimal conditions, the established method presented good linearity (correlation coefficient ≥ 0.9996), precision (relative standard deviation ≤ 13%), accuracy (81-105%), sensitivity (limits of quantification: 4-18 ng kg-1) and extraction performance (10 min).


Assuntos
Ácidos Carboxílicos , Espectrometria de Massas em Tandem , Animais , Ácidos Carboxílicos/análise , Cromatografia Líquida de Alta Pressão/métodos , Cromatografia Gasosa-Espectrometria de Massas/métodos , Metanol/análise , Leite/química , Nylons , Extração em Fase Sólida/métodos , Espectrometria de Massas em Tandem/métodos
14.
J Pharm Anal ; 12(2): 301-307, 2022 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-35582392

RESUMO

Indole-3-carbinol (I3C), an important anticancer compound found in broccoli, has attracted considerable attention. The rapid extraction and accurate analysis of I3C in the pharmaceutical industry in broccoli is challenging as I3C is unstable at low pH and high temperature. In this study, a rapid, accurate, and low-cost ultrasound-assisted dispersive-filter extraction (UADFE) technique based on poly(deep eutectic solvent)-graphene oxide (PDES-GO) adsorbent was developed for the isolation and analysis of I3C in broccoli for the first time. PDES-GO with multiple adsorption interactions and a fast mass transfer rate was synthesized to accelerate adsorption and desorption. UADFE was developed by combining dispersive solid-phase extraction (DSPE) and filter solid-phase extraction (FSPE) to realize rapid extraction and separation. Based on the above two strategies, the proposed PDES-GO-UADFE method coupled with high-performance liquid chromatography (HPLC) allowed the rapid (15-16 min), accurate (84.3%-96.4%), and low-cost (adsorbent: 3.00 mg) analysis of I3C in broccoli and was superior to solid-phase extraction, DSPE, and FSPE methods. The proposed method showed remarkable linearity (r=0.9998; range: 0.0840-48.0 µg/g), low limit of quantification (0.0840 µg/g), and high precision (relative standard deviation ≤5.6%). Therefore, the PDES-GO-UADFE-HPLC method shows significant potential in the field of pharmaceutical analysis for the separation and analysis of anti-cancer compounds in complex plant samples.

15.
Front Nutr ; 9: 862773, 2022.
Artigo em Inglês | MEDLINE | ID: mdl-35520284

RESUMO

Dryopteris crassirhizoma rhizome (DCR) inhibits melanin production in B16F10 melanoma cells and tyrosinase activity. The melanin content and tyrosinase activity of DCR-treated zebrafish embryos were determined to evaluate the in vivo inhibitory effect of DCR on melanogenesis. Moreover, an off-line hyphenated method combining the high-speed counter-current chromatography, affinity-based ultrafiltration, and liquid chromatography-tandem mass spectrometry was used to identify and characterize the DCR compounds with tyrosinase inhibitory activity. Our results indicated that DCR significantly decreased the melanin content and tyrosinase activity in zebrafish embryos in a dose-dependent manner; moreover, 22 compounds in DCR presented tyrosinase inhibitory activity. In silico molecular docking prediction data indicated that the 22 compounds in DCR can form stable conformations in the active site pocket of tyrosinase.

16.
J Chromatogr A ; 1672: 463012, 2022 Jun 07.
Artigo em Inglês | MEDLINE | ID: mdl-35429869

RESUMO

Polychlorinated naphthalenes (PCNs) are emerging organic pollutants that are harmful to the environment and human health. In this study, a headspace solid-phase-microextraction (HS-SPME)-gas chromatography-tandem mass spectrometry method for the separation and enrichment of PCNs in shrimp was developed and validated. A graphene aerogel was prepared by modifying graphene oxide with a deep eutectic solvent to prevent graphene oxide stacking. As a result, the aerogel had a three-dimensional porous structure, which resulted in easy sorption/desorption for PCNs, and was used as the SPME fiber coating. Next, the experimental parameters for the saponification of the sample matrix and the extraction and desorption of the PCNs were systematically optimized. After optimization, the method showed good linearity (R2≥0.9968), low limits of detection (0.00983-0.0661 pg g-1), and satisfactory recoveries (80.4-108%). Crucially, compared with previously reported methods, this method does not require the use of large amounts of organic reagents or complex operations, giving it the advantages of simplicity, sensitivity, and environmental friendliness. As an example of the practical application of the developed method, the PCNs in river and sea shrimp were quantified.


Assuntos
Grafite , Microextração em Fase Sólida , Cromatografia Gasosa-Espectrometria de Massas/métodos , Grafite/química , Humanos , Naftalenos/análise , Microextração em Fase Sólida/métodos , Espectrometria de Massas em Tandem/métodos
17.
Biosens Bioelectron ; 203: 114055, 2022 May 01.
Artigo em Inglês | MEDLINE | ID: mdl-35131695

RESUMO

Protein kinases play crucial regulatory roles in the physiological activities in the human body. Understanding protein kinase activity and its inhibition is essential for the management of human diseases. Considering the limitations of the existing protein kinase-related analysis methods, the aim of the present study was to develop a fluorescent biosensor based on Eu(BTC) (H2O)6 (BTC = 1,3,5-Benzenetricarboxylic acid) for evaluating protein kinase activity and the relevant inhibitors. A fluorophore-labelled substrate polypeptide was phosphorylated under the catalysis of protein kinase. This phosphorylated peptide can be coordinated explicitly with the europium site of Eu(BTC) (H2O)6 to detect the protein kinase. The developed biosensor performed well, with a detection limit of 0.00003 U µL-1, and it showed good selectivity and universality. Protein kinase activity could also be detected in MCF-7 cells using this method. Furthermore, in terms of inhibitor screening using the Eu(BTC) (H2O)6-based sensor, both H-89 and ellagic acid were found to inhibit protein kinase activity with IC50 values of 1.09 and 19.88 nmol L-1, respectively. Overall, this biosensor has broad application prospects in monitoring and controlling protein kinase activity.


Assuntos
Técnicas Biossensoriais , Estruturas Metalorgânicas , Técnicas Biossensoriais/métodos , Európio , Fosforilação , Proteínas Quinases/metabolismo
18.
Foods ; 10(3)2021 Mar 05.
Artigo em Inglês | MEDLINE | ID: mdl-33807644

RESUMO

The defatted seeds of Oenothera biennis (DSOB) are a by-product of evening primrose oil production that are currently not effectively used. In this study, α-glucosidase inhibition, aldose reductase inhibition, antioxidant capacity, polyphenol composition, and nutritional value (carbohydrates, proteins, minerals, fat, organic acid, and tocopherols) of DSOB were evaluated using the seeds of Oenothera biennis (SOB) as a reference. DSOB was an excellent inhibitor of α-glucosidase (IC50 = 3.31 µg/mL) and aldose reductase (IC50 = 2.56 µg/mL). DSOB also showed considerable antioxidant capacities (scavenging of 2,2-diphenyl-1-picrylhydrazyl, 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid, nitric oxide, peroxynitrite, and hydroxyl radicals). DSOB was a reservoir of polyphenols, and 25 compounds in DSOB were temporarily identified by liquid chromatography coupled with electrospray ionization-quadrupole time of flight-mass spectrometry analysis. Moreover, the carbohydrate, protein, and mineral content of DSOB were increased compared to that of SOB. DSOB contained large amounts of fiber and low levels of sugars, and was rich in calcium and iron. These results imply that DSOB may be a potential functional food ingredient for diabetes, providing excellent economic and environmental benefits.

19.
Food Chem ; 349: 128982, 2021 Jul 01.
Artigo em Inglês | MEDLINE | ID: mdl-33561797

RESUMO

This paper reports a selective, sensitive, and miniaturized analytical method based on a molecularly imprinted graphene oxide (MIP-GO) composite as adsorbent for miniaturized tip solid-phase extraction (MTSPE) to determine naphthalene-derived plant growth regulators (PGRs) in apples. The proposed method combines the advantages of MIP-GOs (high selectivity), MTSPE (low consumption), and high-performance liquid chromatography-fluorescence detection (high sensitivity). Under optimized conditions, the method exhibited appreciable linearity (2.00-200 ng/g), low detection limits (0.21-0.53 ng/g), high accuracy (absolute recoveries: 87.6-99.5%), and high precision (relative standard deviations ≤ 3.0%), along with low consumption (0.5 mL sample solution and 2.0 mg adsorbent). In addition, the adsorption performance of the MIP-GO adsorbent did not decrease over ten months, highlighting the long storage and operational lifetime of the adsorbent. The proposed method was employed for the analysis of naphthalene-derived PGR residues in apples and exhibited promising potential for application in food safety analysis.


Assuntos
Análise de Alimentos/métodos , Grafite/química , Malus/química , Impressão Molecular , Naftalenos/química , Reguladores de Crescimento de Plantas/análise , Reguladores de Crescimento de Plantas/química , Adsorção , Cromatografia Líquida de Alta Pressão , Limite de Detecção , Extração em Fase Sólida/métodos , Fatores de Tempo
20.
Chem Asian J ; 16(2): 114-128, 2021 Jan 18.
Artigo em Inglês | MEDLINE | ID: mdl-33289286

RESUMO

MicroRNA (miRNA) is an important tumor marker in the human body, and its early detection has a great influence on the survival rate of patients. Although there are many detection methods for miRNA at present such as northern blotting, real-time quantitative polymerase chain reaction, microarrays, and others, electrochemical biosensors have the advantages of low detection cost, small instrument size, simple operation, non-invasive detection and low consumption of reagents and solvents, and thus they play an important role in the early detection of cancer. In addition, with the development of nanotechnology, nano-biosensors show great potential. The application of various nanomaterials in the development of electrochemical biosensor has greatly improved the detection sensitivity of electrochemical biosensor. Among them, carbon nanomaterials which have unique electrical, optical, physical and chemical properties have attracted increasing attention. In particular, they have a large surface area, good biocompatibility and conductivity. Therefore, carbon nanomaterials combined with electrochemical methods can be used to detect miRNA quickly, easily and sensitively. In this review, we systematically review recent applications of different carbon nanomaterials (carbon nanotubes, graphene and its derivatives, graphitic carbon nitride, carbon dots, graphene quantum dots and other carbon nanomaterials) for miRNA electrochemical detection. In addition, we demonstrate the future prospects of electrochemical biosensors modified by carbon nanomaterials for the detection of miRNAs, and some suggestions for their development in the near future.


Assuntos
MicroRNAs/sangue , Nanotubos de Carbono/química , Pontos Quânticos/química , Biomarcadores Tumorais/sangue , Biomarcadores Tumorais/genética , Técnicas Biossensoriais/métodos , Sondas de DNA/química , Sondas de DNA/genética , Técnicas Eletroquímicas/métodos , Grafite/química , Humanos , Ácidos Nucleicos Imobilizados/química , Ácidos Nucleicos Imobilizados/genética , MicroRNAs/genética , Neoplasias/diagnóstico , Compostos de Nitrogênio/química , Hibridização de Ácido Nucleico
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