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1.
Food Chem ; 450: 139341, 2024 Apr 16.
Artigo em Inglês | MEDLINE | ID: mdl-38631206

RESUMO

The escalating use of pesticides on fruits and vegetables has raised concerns about potential health risks. Therefore, we developed a superhydrophilic resin/graphene oxide (SR/GO) with rich adsorption interactions using an eco-friendly synthetic approach. SR/GO demonstrated excellent hydrophilicity, ensuring optimal contact with aqueous sample matrices. The multiple adsorption interactions, including π-π conjugation, hydrogen bonding, and electrostatic adsorption, facilitated multi-pesticide residue co-extraction. The synthesized SR/GO was applied to a miniaturized centrifugation-accelerated pipette-tip extraction method, coupled with high-performance liquid chromatography. The optimized method exhibited low consumption (15.0 mg adsorbent), and high efficiency, with low detection limits (1.4-2.9 ng g-1) and high recoveries (75.3-113.0%). Water-compatible SR/GO, along with a miniaturized extraction process, showcases a potent analytical approach for pesticide residue analysis in fruits and vegetables. The significance of this method lies in its ability to ensure agricultural and food safety by using a low-cost and efficient multi-pesticide residue analytical strategy.

2.
Talanta ; 275: 126017, 2024 Apr 04.
Artigo em Inglês | MEDLINE | ID: mdl-38626499

RESUMO

It is extremely significant while challenging to accurately detect low-levels of perfluoroalkyl carboxylic acid compounds (PFCAs) in environmental water. Herein, adopting perfluorotetradecanoic acid as the dummy template, selective molecularly imprinted composites (CNTs@ILs@MIPs) grafted carbon nanotubes integrating hydrophilic ionic liquids were successfully prepared via surface imprinting and dummy-template imprinting techniques. The obtained CNTs@ILs@MIPs were applied as selective extraction adsorbent for specifically extract PFCAs in environmental water coupled with gas chromatography-mass spectrometry quantification. Detailed studies were conducted on the main preparation parameters and extraction conditions. The CNTs@ILs@MIPs displayed excellent adsorptivity, and the established method exhibited low LODs (0.60-1.64 ng L-1), wide linearity with R2 above 0.9994, and satisfactory adsorption recoveries (80.5-112.5%) for seven PFCAs. This proposed method provides a new applicable approach for the detection of targeted pollutants in environmental water by utilizing the high affinity and recognition ability of molecularly imprinted carbon nanotube functional materials modified with ionic liquids.

3.
Talanta ; 274: 125913, 2024 Mar 24.
Artigo em Inglês | MEDLINE | ID: mdl-38547839

RESUMO

In this study, a novel three-dimensional hierarchical porous deep eutectic solvents-modified graphene aerogel (3D DES-GA) was synthesized for use as a solid-phase microextraction (SPME) fiber coating. The SPME fiber was characterized by its fluffy and hierarchical porous structure, uniform thickness, and rapid mass transfer capabilities. This fiber demonstrated a lifetime (≥160 uses) and excellent precision (with relative standard deviations of 2.4-6.6% for single fiber and 6.0-9.8% for fiber-to-fiber repeatability). The SPME fiber also exhibited remarkable extraction performance for polycyclic aromatic hydrocarbons and polychlorinated biphenyls, which are common persistent organic pollutants in environmental samples. When combined with gas chromatography-tandem mass spectrometry, the method allowed for high-efficiency extraction (enrichment factors ranging from 1225 to 4652 folds) and sensitive determination (limit of detection ranging from 0.010 to 0.056 pg g-1) of polychlorinated naphthalenes (PCNs) in complex samples. To validate this method, we applied it to the determination of four PCNs in five types of fish tissues. The results revealed the presence of 1-chloronaphthalene at concentrations of 7.0 ± 2.9-34.8 ± 2.1 pg g-1 and 1,4-dichloronaphthalene at concentrations of 6.0 ± 0.3-10.9 ± 1.4 pg g-1 in three fish species. Compared with reported sample pretreatment methods reported in the literature, this proposed headspace SPME method offers additional advantages, including simplicity of operation and reduced sample and organic solvent consumption.

4.
J Hazard Mater ; 469: 133909, 2024 May 05.
Artigo em Inglês | MEDLINE | ID: mdl-38432094

RESUMO

The residues of polychlorinated naphthalenes (PCNs) produced in multiple industrial production and life processes are continuously entering environmental waters through atmospheric deposition and land drainage, and the water pollution caused by PCNs is continuing public concern due to their potential threat to aquatic ecosystems and public health. Herein, a new chlorine-functionalized covalent organic framework anchored graphene aerogel (COF-GA) was synthesized by covalent modification technology and used as fiber coating of solid-phase microextraction for synergically enhanced extraction of PCNs in environmental water. The extraction efficiency of COF-GA coated fiber was superior to commercial fiber due to the multiple interactions (π-π, hydrophobic interaction, and halogen bonding interaction). The COF-GA coated fiber has good stability, can avoid water vapor interference at 80 °C for a long time (30 -50 min) to maintain adsorption equilibrium, and can be reused at least 96 times. Combined with gas chromatography-tandem mass spectrometry, a sensitive method for the high-efficient enrichment (enrichment factors were 501 -7453 folds) and ultra-sensitive detection (LODs were 0.001 -0.428 pg/mL) of PCNs in environmental water was established. The enrichment factor for PCNs is significantly higher than in previous studies. This proposed method provides new technical support for the daily monitoring and risk assessment of trace PCNs in environmental water.

5.
Food Res Int ; 180: 114097, 2024 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-38395549

RESUMO

The defatted seeds of evening primrose (DE), a by-product of evening primrose oil extraction, are currently underutilized. This study aimed to valorize DE by examining its effects on melanogenesis and tyrosinase activity in zebrafish embryos and in vitro, and an innovative affinity-labeled molecular networking workflow was proposed for the rapid identification of tyrosinase inhibitors in DE. Our results indicated DE significantly reduced melanin content (53.3 % at 100 µg/mL) and tyrosinse activity (80.05 % for monophenolase and 70.40 % for diphenolase at 100 µg/mL). Furthermore, through the affinity-labeled molecular networking approach, 20 compounds were identified as potential tyrosinase inhibitors within DE, predominantly flavonoids and tannins characterized by catechin and galloyl substructures. Seven of these compounds were isolated and their inhibitory effects on tyrosinase were validated using functional assays. This study not only underscores the potential of DE as a rich source of natural tyrosinase inhibitors but also establishes the effectiveness of affinity-labeled molecular networking in pinpointing bioactive compounds in complex biological matrices.


Assuntos
Oenothera biennis , Animais , Oenothera biennis/química , Monofenol Mono-Oxigenase , Peixe-Zebra , Extratos Vegetais/farmacologia , Flavonoides/farmacologia
6.
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
7.
Talanta ; 270: 125620, 2024 Apr 01.
Artigo em Inglês | MEDLINE | ID: mdl-38176249

RESUMO

Efficiently detecting diamide insecticides in environmental water is challenging due to their low concentrations and complex matrix interferences. In this study, we developed ionic liquids (ILs)-incorporated magnetic molecularly imprinted polymers (IL-MMIPs) for the detection of diamide insecticides, capitalizing on the advantages of ILs and quick magnetic separation through surface imprinting. Tetrachlorantraniliprole was used as the template, and a specific IL, 1-vinyl-3-ethylimidazolium hexafluorophosphate ([VEIm][PF6]), was employed as the functional monomer. Various synthesis conditions were investigated to optimize adsorption efficiency. The prepared IL-MMIPs were successfully employed as adsorbents in magnetic solid-phase extraction (MSPE) to selectively extract, separate, and quantify three types of diamide insecticides from water samples using HPLC-UV detection. Under optimal conditions, the analytical method achieved low limits of detection (0.69 ng mL-1, 0.64 ng mL-1, 0.59 ng mL-1 for cyantraniliprole, chlorantraniliprole and tetrachlorantraniliprole, respectively). The method also displayed a wide linear range (0.003-10 µg mL-1 for cyantraniliprole and chlorantraniliprole, and 0.004-10 µg mL-1 for tetrachlorantraniliprole, respectively) with satisfactory coefficients (R2≥0.9996), and low relative standard deviation (RSD≤2.55%). Additionally, extraction recoveries fell within the range of 79.4%-109%. The results clearly demonstrate that IL-MMIPs exhibit exceptional recognition and rebinding capabilities. The developed IL-MMIPs-MSPE-HPLC-UV method is straightforward and rapid, making it suitable for the detection and analysis of three kinds of diamide insecticides in environmental water.


Assuntos
Inseticidas , Líquidos Iônicos , Impressão Molecular , Pirazóis , ortoaminobenzoatos , Água , Polímeros Molecularmente Impressos , Diamida , Impressão Molecular/métodos , Cromatografia Líquida de Alta Pressão , Polímeros , Adsorção , Fenômenos Magnéticos , Extração em Fase Sólida/métodos
8.
Talanta ; 271: 125711, 2024 May 01.
Artigo em Inglês | MEDLINE | ID: mdl-38290266

RESUMO

The three-dimensional porous ionic liquid-chitosan-graphene oxide aerogel (IL-CS-GOA) monolithic adsorbent with a through-hole structure was prepared using natural chitosan (CS) as the skeletal framework, graphene oxide (GO) as the support to provide mechanical strength, and ionic liquid (IL) as the porogen and modifier. The resulting IL-CS-GOA demonstrated a fluffy and porous structure with various pore sizes and excellent regeneration capability (over six cycles). Its specific surface area exceeded that of CS-GOA and IL-GOA by more than 7 times, enhancing its polyhalogenated carbazoles (PHCZs) adsorption capacity. Within 5 min, IL-CS-GOA (1.0 mg) exhibited adsorption amounts of 539 ng mg-1 for 3-bromocarbazole (3-BCZ), 716 ng mg-1 for 2,7-dibromocarbazole (2,7-BCZ), and 798 ng mg-1 for 1,3,6,8-tetrabromocarbazole (1,3,6,8-BCZ), showcasing its rapid mass transfer and high adsorption capabilities. IL-CS-GOA was utilized as the adsorbent for glass dropper extraction (GDE) in conjunction with gas chromatography-mass spectrometry (GC-MS/MS), to develop a highly efficient and accurate method for determining PHCZs in sediments. Under optimal conditions, the established method exhibited a wide linear range (0.4-250 ng g-1, r ≥ 0.9990), low detection limits (0.04-0.24 ng g-1), and satisfactory recoveries (80.5 %-93.8 %), enabling the accurate and rapid detection of PHCZs in sediment samples. This study presents a novel approach for creating three-dimensional porous aerogels, introduces a new form of sample pretreatment using GDE with a monolithic adsorbent, and offers a new method for the determination of PHCZs in environmental matrices.

9.
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
10.
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
11.
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
12.
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
13.
J Pharm Biomed Anal ; 234: 115508, 2023 Sep 20.
Artigo em Inglês | MEDLINE | ID: mdl-37295190

RESUMO

Natural glycosides widely distributed in medicinal plants are valuable sources of therapeutic agents, showing various pharmacological effects. The separation and purification of natural glycosides are meaningful for their pharmacological research, which face with great challenges due to the complex of medicinal plants samples. In this work, two kinds of functional monolithic separation mediums A and S were fabricated and fully applied in the online extraction, separation and purification of active glycoside components from medicinal plants with a simple-procedure closed-loop mode. Chrysophanol glucoside and physcion glucoside were detected and separated from Rhei Radix et Rhizoma using separation medium A as a solid-phase extraction adsorbent. Rhapontin was isolated and purified from Rheum hotaoense C. Y. Cheng et Kao using separation medium S as the stationary phase of high-performance liquid chromatography. Compared to the reported literatures, high yield of 5.68, 1.20 and 4.76 mg g-1 of these three products were obtained with high purity. These two online closed-loop mode methods were carried out using high-performance liquid chromatography system, in which the sample injection, isolation and purification procedures are all online mode, and reduced loss compared to offline extraction and purification procedures, thus achieving high recovery and high purity.


Assuntos
Medicamentos de Ervas Chinesas , Plantas Medicinais , Rheum , Plantas Medicinais/química , Glicosídeos/análise , Medicamentos de Ervas Chinesas/química , Rizoma/química , Cromatografia Líquida de Alta Pressão/métodos , Glucosídeos/análise , Rheum/química
14.
Anal Chim Acta ; 1269: 341404, 2023 Aug 15.
Artigo em Inglês | MEDLINE | ID: mdl-37290858

RESUMO

Dopamine (DA) and l-tyrosine (l-Tyr) are neurotransmitters involved in various neuropsychiatric disorders. Therefore, it is important to monitor their levels for diagnosis and treatment. In this study, we synthesized poly (methacrylic acid)/graphene oxide aerogels (p(MAA)/GOA) by in situ polymerization and freeze-drying using graphene oxide and methacrylic acid as substrates. Then, the p(MAA)/GOA were applied as solid-phase extraction adsorbents to extract DA and l-Tyr from urine samples, followed by quantification using high performance liquid chromatography (HPLC). The p(MAA)/GOA showed better adsorption performance for DA and l-Tyr than commercial adsorbents, likely as a result of the strong adsorption of the target analytes via π-π and hydrogen bonding interactions. Further, the developed method had good linearity (r > 0.9990) at concentrations of DA and l-Tyr of 0.075-2.0 and 0.75-20.0 µg mL-1, respectively, as well as a limit of detection of 0.018-0.048 µg mL-1, limit of quantitation of 0.059-0.161 µg mL-1, spiked recovery of 91.1-104.0%, and interday precision of 3.58-7.30%.The method was successfully applied to determine DA and l-Tyr in the urine samples of patients suffering from depression, demonstrating its potential for clinical applications.


Assuntos
Dopamina , Tirosina , Humanos , Depressão/diagnóstico , Limite de Detecção , Extração em Fase Sólida/métodos , Cromatografia Líquida de Alta Pressão/métodos
15.
J Chromatogr A ; 1702: 464087, 2023 Aug 02.
Artigo em Inglês | MEDLINE | ID: mdl-37230054

RESUMO

In this work, a series of 5,10,15,20-tetraphenylporphyrin (TPP)-based hyper crosslinked polymers were prepared by Friedel-Crafts reaction. Among them, the HCP-TPP-BCMBP, which was prepared by using TPP as the monomer and with 4,4'-Bis(chloromethyl)-1,1'-biphenyl (BCMBP) as the cross-linking agent, had the best adsorption capability for the enrichment of the nitroimidazoles of dimetridazole, ronidazole, secnidazole, metronidazole, and ornidazole. Then, a solid-phase extraction (SPE) method with the HCP-TPP-BCMBP as adsorbent coupled with HPLC-UV detection for the determination of nitroimidazole residues in honey, environmental water, and chicken breast samples was established. The influence of the main factors that affect the SPE, i.e., sample solution volume, sample loading rate, sample pH, and eluent and its volume, were studied. Under the optimal conditions, the limits of detection (S/N = 3) for the nitroimidazoles were measured to be in the range of 0.02-0.04 ng mL-1, 0.4-1.0 ng g-1 and 0.5-0.7 ng g-1 for environmental water, honey, and chicken breast samples, with the determination coefficients being in the range of 0.9933-0.9998. The analytes recoveries by the method in fortified samples fell in the range from 91.1% to 102.7% for environmental water, from 83.2% to 105.0% for honey, and from 85.9% to 103.0% for chicken breast samples, and the relative standard deviations for the determination were less than 10%. It shows that the HCP-TPP-BCMBP has a strong adsorption capability for some polar compounds.


Assuntos
Mel , Nitroimidazóis , Animais , Nitroimidazóis/análise , Galinhas , Água , Mel/análise , Polímeros/química , Cromatografia Líquida de Alta Pressão/métodos , Extração em Fase Sólida/métodos , Limite de Detecção
16.
Anal Chim Acta ; 1260: 341222, 2023 Jun 15.
Artigo em Inglês | MEDLINE | ID: mdl-37121655

RESUMO

Triazine herbicides have been widely detected in water resources and food, which poses a potential hazard to both ecosystem and human health. Due to their high polarity, conventional adsorbents have limitations for their extractions. Herein, for the effective magnetic extraction of triazine herbicides, a novel and effective magnetic adsorbent was prepared with a satisfactory extraction performance. In the experiments, five porous organic frameworks (POFs) with hydroxyl functional groups were synthesized by diazo-coupling reactions in aqueous solution with ß-cyclodextrin (ß-CD) as a green monomer. After evaluation of the five POFs, the DDM-CD-POF, which was synthesized with 4'4-diaminodiphenylmethane (DDM) and ß-CD, showed the largest specific surface area and the best adsorption capacity for the five triazine herbicides. Then, it was magnetized by introducing Fe3O4@SiO2 into it to prepare a magnetic adsorbent (M-DDM-CD-POF) to facilitate separation and recycling. Finally, the M-DDM-CD-POF-based magnetic solid-phase extraction in combination with high performance liquid chromatographic detection method was established for the quantitative determination of the triazine herbicides in environmental water and watermelon juice samples. The current strategy showed low limits of detection of 0.03-0.11 ng mL-1 for environmental water and 0.07-0.22 ng mL-1 for watermelon juice sample. The method recoveries for spiked samples ranged from 84.0% to 113.0% with the relative standard deviations ≤8.8%. This work provides a new approach for the detection of the triazine herbicides with good application prospect.


Assuntos
Herbicidas , Água , Humanos , Cromatografia Líquida de Alta Pressão , Ecossistema , Herbicidas/análise , Limite de Detecção , Fenômenos Magnéticos , Porosidade , Dióxido de Silício , Extração em Fase Sólida/métodos , Triazinas/química , Bebidas
17.
J Chromatogr A ; 1695: 463956, 2023 Apr 26.
Artigo em Inglês | MEDLINE | ID: mdl-37019061

RESUMO

A new strategy has been developed to fabricate a bovine haemoglobin surface-imprinted core-shell nanocomposite adsorbent, demonstrating superparamagnetism via emulsion-free and sol-gel techniques. The obtained magnetic surface-imprinted polymers (MSIPs) possess a porous core-shell nanocomposite structure with a remarkable imprinted recognition ability for template protein in aqueous medium. The MSIPs display higher affinity, adsorption efficiency and selectivity, for template protein compared to the non-target protein. The morphology, adsorption, and recognition properties of the MSIPs have been evaluated by using several characterisation techniques, such as scanning electron microscopy, transmission electron microscopy, X-ray powder diffraction, Fourier transform infrared spectroscopy, thermogravimetric analysis, and vibrating sample magnetometry. The results show the average diameter of MSIPs ranging between 400 and 600 nm with a saturation magnetization value of 52.6 emu/g and adsorption capacity of 43.75 mg/g. And because the obtained MSIPs possessed easily accessible recognition sites and performed fast kinetics for template immobilization, it could achieve equilibrium within 60 min. All this revealed the potential application of this approach as an alternative methodology for the generation of protein imprinted biomaterials.


Assuntos
Nanopartículas de Magnetita , Impressão Molecular , Nanocompostos , Bovinos , Animais , Polimerização , Impressão Molecular/métodos , Hemoglobinas/química , Polímeros/química , Adsorção , Nanopartículas de Magnetita/química
18.
Food Chem ; 411: 135471, 2023 Jun 15.
Artigo em Inglês | MEDLINE | ID: mdl-36669342

RESUMO

In recent years, numerous plant growth regulators have been found in foods and have a toxicity to human health, so its simultaneous multiple monitoring is urgently. For the first time, a rapid, accurate, and high-selective method was established to extract and determine multiple plant growth regulators simultaneously in red wines using a new dual-template hydrophilic molecularly imprinted resin (DHMIR) as an adsorbent of pipette tip solid-phase extraction coupled with HPLC. The as-prepared DHMIR combined the advantages of the hydrophilicity of hydrophilic resin and multi-imprinted recognition of dual-template molecular imprinting, overcoming the poor imprinted recognition ability of traditional imprinting materials in water and low extraction efficiency to multiple targets. Under the optimized conditions, the proposed method exhibited high sensitivity (2.29-3.94 ng mL-1) and recoveries (80.9-109.0 %) using only 15 mg DHMIR. This study provides an effective strategy for rapid, accurate, low-cost, and high-selective determination of the multiple analytes in food samples.


Assuntos
Impressão Molecular , Vinho , Humanos , Reguladores de Crescimento de Plantas/análise , Cromatografia Líquida de Alta Pressão/métodos , Água , Interações Hidrofóbicas e Hidrofílicas , Impressão Molecular/métodos , Extração em Fase Sólida/métodos
19.
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
20.
ACS Appl Mater Interfaces ; 15(5): 6338-6353, 2023 Feb 08.
Artigo em Inglês | MEDLINE | ID: mdl-36701257

RESUMO

Bacteria-infected skin wounds caused by external injuries remain a serious challenge to the whole society. Wound healing dressings, with excellent antibacterial activities and potent regeneration capability, are increasingly needed clinically. Here, we reported a novel functional microneedle (MN) array comprising methacrylated hyaluronic acid (MeHA) embedded with pH-responsive functionalized zeolitic imidazolate framework-8 (ZIF-8) nanoparticles to treat bacteria-infected cutaneous wounds. Antibacterial activity was introduced into Zn-ZIF-8 to achieve sterilization through releasing Zn ions, as well as increased angiogenesis by dimethyloxalylglycine (DMOG) molecules that were distributed within its framework. Furthermore, biodegradable MeHA was chosen as a substrate material carrier to fabricate DMOG@ZIF-8 MN arrays. By such design, DMOG@ZIF-8 MN arrays would not only exhibit excellent antibacterial activity against pathogenic bacteria but also enhance angiogenesis within wound bed by upregulating the expression of HIF-1α, leading to a significant therapeutic efficiency on bacteria-infected cutaneous wound healing. Based on these results, we conclude that this new treatment strategy can provide a promising alternative for accelerating infected wound healing via effective antibacterial activity and ameliorative angiogenesis.


Assuntos
Sistemas de Liberação de Medicamentos , Nanopartículas , Zeolitas , Antibacterianos/administração & dosagem , Antibacterianos/farmacologia , Bactérias , Nanopartículas/química , Zeolitas/química , Cicatrização
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