RESUMO
In this work, a novel extraction technique based on the effervescence-assisted dispersion and magnetic recovery of attapulgite/polypyrrole sorbents was developed for determining the concentrations of five pyrethroids in honey samples. The magnetic nanoparticles were synthesized by a one-pot method. Several experimental parameters that affected the extraction efficiency, including the dispersion conditions, pH, ionic strength, and desorption conditions, were investigated. Under optimal conditions, the calibration curves for the five pyrethroids in honey samples exhibited good linearity, with r2 values ranging from 0.9979 to 0.9990. The limits of detection varied between 0.21 and 0.34 µg/L. Satisfactory recoveries of 81.42-106.73% with intra- and interday relative standard deviations of less than 6.94 and 10.89%, respectively, were obtained. Moreover, the sorbents exhibited acceptable batch-to-batch repeatability in the range of 5.06-15.01%, and each sorbent could be reused for up to four extraction cycles without a significant loss in the extraction recovery.
Assuntos
Mel/análise , Compostos de Magnésio/química , Nanocompostos/química , Polímeros/química , Piretrinas/análise , Pirróis/química , Compostos de Silício/química , Extração em Fase Sólida , Adsorção , Fenômenos Magnéticos , Tamanho da Partícula , Propriedades de SuperfícieRESUMO
Hyperbranched polytriazine functionalized with humic acid was prepared and developed as new sorbents for dispersive solid-phase extraction of three acaricides (clofentezine, fenpyroximate, and pyridaben) in tea samples combined with high-performance liquid chromatography detection. The sorbents were characterized by scanning electron microscopy, energy dispersive spectroscopy, Zeta-potential, and Fourier transform infrared spectroscopy. The extraction parameters (extraction time, ionic strength, desorption conditions) were optimized. The adsorption mechanism was evaluated utilizing Fourier transform infrared spectra. Under optimum conditions, satisfactory analytical performances were achieved, which included high precision (1.33-9.62%), low limits of detection (0.19-3.54⯵g/L), and wide linear range (2.5-500⯵g/L) for the analysis of the acaricides. Moreover, the proposed method proved highly effective for the determination of acaricides in tea samples, with the relative recoveries in the range of 65.20-108.13% and relative standard deviations < 9.87%. The method has great application potential for the detection of acaricides in tea samples.
Assuntos
Acaricidas/análise , Substâncias Húmicas/análise , Polímeros/química , Extração em Fase Sólida , Chá/química , Triazinas/química , Estrutura Molecular , Tamanho da Partícula , Propriedades de SuperfícieRESUMO
Allatostatins (AST) are neuropeptides originally described as inhibitors of juvenile hormone (JH) synthesis in insects. Consequently, they have been considered as potential lead compounds for the discovery of new insect growth regulators (IGRs). In the present work, receptor-based three-dimensional quantitative structure-activity relationship (3D-QSAR) was studied with 48 AST analogs, and a general approach for novel potent bioactive AST analogs is proposed. Hence, six novel AST analogs were designed and synthesized. Bioassays indicated that the majority novel analogs exhibited potent JH inhibitory activity, especially analog A6 (IC50: 3.79â¯nmol/L), which can be used as lead compound to develop new IGRs.
Assuntos
Proteínas de Insetos/química , Hormônios Juvenis/química , Neuropeptídeos/química , Animais , Sítios de Ligação , Baratas/química , Proteínas de Insetos/síntese química , Proteínas de Insetos/metabolismo , Hormônios Juvenis/antagonistas & inibidores , Hormônios Juvenis/metabolismo , Simulação de Acoplamento Molecular , Estrutura Molecular , Neuropeptídeos/síntese química , Neuropeptídeos/metabolismo , Ligação Proteica , Relação Quantitativa Estrutura-Atividade , Receptores de Neuropeptídeos/química , Receptores de Neuropeptídeos/metabolismoRESUMO
In this study, a novel ionic liquid-type surfactant modified attapulgite named as 1-dodecyl-3-methylimidazolium bromide-attapulgite (C12MIM-ATP) is successfully prepared and applied in dispersive solid phase extraction (dSPE) for the fast determination of pyrethroid residues in tea drinks. The primary factors that influenced the extraction efficiency, including sorbent type, amount of sorbent, extraction time, desorption conditions, pH and ionic strength, are investigated. The optimized results reveal that the extraction and desorption equilibria are rapidly obtained within 1â¯min. Under the optimized conditions, good linearity (2-500⯵g/L) is observed for four pyrethroids in tea drinks with determination coefficients (r2) ranged from 0.9992 to 1.0000. The limits of detection (LODs) are 0.6⯵g/L for all pesticides. Acceptable extraction recoveries of target analytes are found from 90.28 to 107.56% with relative standard deviations (RSDs) less than 8.30% in real tea drink samples. The batch-to-bath repeatability is evaluated by recovery test on five independent synthesized C12MIM-ATP sorbents. Satisfactory batch-to-batch repeatability is obtained with the recovery factors varied in 15%. A small matrix effect is observed using C12MIM-ATP as the sorbent for detection pyrethroids in tea drinks.