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1.
J Chromatogr A ; 1689: 463744, 2023 Jan 25.
Artigo em Inglês | MEDLINE | ID: mdl-36610187

RESUMO

In food safety monitoring, on-site and simultaneous detection of a variety of insecticides with different concentrations in the same matrix is necessary. However, the task remains challenging. In this study, a novel nitrogen and sulfur co-doped carbon dot (N, S-CD) was synthesized and used as a QuEChERS clean-up reagent to reduce matrix interferences in the determination of insecticides in vegetables. In addition, a portable mass spectrometer (µ-MS) was employed, without chromatography separation, to directly determine neonicotinoids, carbamates, and benzopyrazole insecticides (with acetamiprid, imidacloprid, thiamethoxam, fipronil, and carbofuran as models) in the pretreated samples. The N,S-CD µ-MS method exhibited effective clean-up performance with satisfactory matrix effects between -15.2% and 15.7%. The recoveries of spiked vegetable samples ranged from 82.2% to 109.7% for the five target insecticides, and the relative standard deviations (RSDs) ranged from 3.8% to 16.5%. The linear ranges were from 2.0 to 5.0 ng/g, with low detection limits (LOD) from 0.5 to 1.0 ng/g. Moreover, the total pretreatment and detection time was within 20 min. Thus, the incorporation of N,S-CD with QuEChERS extraction, together with the portable µ-MS system, could be a promising and feasible strategy for on-site, rapid, and simultaneous detection of various insecticides in vegetables.


Assuntos
Inseticidas , Resíduos de Praguicidas , Inseticidas/análise , Verduras/química , Carbamatos/análise , Espectrometria de Massas em Tandem/métodos , Neonicotinoides/análise , Pirazóis , Resíduos de Praguicidas/análise , Cromatografia Líquida de Alta Pressão/métodos
2.
Anal Chim Acta ; 1225: 340199, 2022 Sep 08.
Artigo em Inglês | MEDLINE | ID: mdl-36038230

RESUMO

Degradation analysis of therapeutic mAb is of high interest for critical quality attributes assessment and biotransformation studies. However, some obstacles, including low in vivo concentrations of mAb and complex biological matrices containing IgGs, could seriously interfere with mAb bioanalysis. In this study, a bioanalytical platform was developed for studying in vitro/in vivo modifications of trastuzumab, in which specific capture on mimotope peptide modified material was combined with trypsin digestion and LC-QTOF-MS analysis. It is worth noting that this material exhibits high specificity, suitable dynamic binding capacity, very little non-specific protein adsorption, and thus provides good enrichment and quantification performances for trastuzumab from patient serums. In particular, this bioanalytical platform was successfully applied to the dynamic monitoring of modifications of trastuzumab, such as deamidation, isomerization, oxidation and cyclization. Except for the faster deamidation of LC-Asn-30 and HC-Asn-387/392/393 under serum incubation, similar degradation trends for other sites were observed in phosphate buffer and spiked serum. Differences of peptide modification degrees of trastuzumab in patient serums were also observed. The novel platform exhibited superior specificity than Protein A/G/L based analytical methods, lower cost and higher stability than antigen or anti-idiotypic antibody based analytical methods, ensuring the evaluation of modification sites.


Assuntos
Anticorpos Monoclonais , Espectrometria de Massas em Tandem , Cromatografia Líquida/métodos , Humanos , Peptídeos , Espectrometria de Massas em Tandem/métodos , Trastuzumab
3.
Beilstein J Nanotechnol ; 10: 1157-1165, 2019.
Artigo em Inglês | MEDLINE | ID: mdl-31293853

RESUMO

A mild and simple method was developed to synthesize a highly efficient photocatalyst comprised of Ce-doped ZnO rods and optimal synthesis conditions were determined by testing samples with different Ce/ZnO molar ratios calcined at 500 °C for 3 hours via a one-step pyrolysis method. The photocatalytic activity was assessed by the degradation of a common dye pollutant found in wastewater, rhodamine B (RhB), using a sunlight simulator. The results showed that ZnO doped with 3% Ce exhibits the highest RhB degradation rate. To understand the crystal structure, elemental state, surface morphology and chemical composition, the photocatalysts were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscope (SEM) and inductively coupled plasma emission spectroscopy (ICP), respectively. The newly developed, robust, field-only surface integral method was employed to explore the relationship between the remarkable catalytic effect and the catalyst shape and porous microstructure. The computational results showed that the dipole-like field covers the entire surface of the rod-like Ce-doped ZnO photocatalyst and is present over the entire range of wavelengths considered. The optimum degradation conditions were determined by orthogonal tests and range analysis, including the concentration of RhB and catalyst, pH value and temperature. The results indicate that the pH value is the main influential factor in the photocatalytic degradation process and the optimal experimental conditions to achieve the maximum degradation rate of 97.66% in 2 hours are as follows: concentration (RhB) = 10 mg/L, concentration (catalyst) = 0.7 g/L, pH 9.0 and T = 50 °C. These optimum conditions supply a helpful reference for large-scale wastewater degradation containing the common water contaminant RhB.

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