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1.
J Chromatogr A ; 1706: 464220, 2023 Sep 13.
Artigo em Inglês | MEDLINE | ID: mdl-37523906

RESUMO

In this work, for the first time, magnetic-phthalated maltodextrin nanosponges (M-PAMDNSs) were synthetized and introduced as efficient and green sorbents. The integration of phthaloyl groups as hydrophobic moieties into networks of maltodextrin nanosponges provided good enrichment for hypothalamic-related peptides (HRPs). The synthesized materials were characterized by 1H nuclear magnetic resonance spectroscopy, water contact angle, attenuated total reflection-Fourier transform infrared spectroscopy, dynamic light scattering, zeta potential, pH point of zero charge, acid-base titration, field-emission scanning electron microscopy, Brunauer-Emmett-Teller, and vibrating sample magnetometer. Under the optimized conditions (sorbent amount: 5.0 mg, desorption solvent volume and type: 300 µL of methanol: H2O: trifluoroacetic acid, extraction time: 15 min, and desorption time: 10 min), the developed magnetic solid-phase extraction (MSPE) method in combination with HPLC-UV was used as a novel and sensitive analytical method for the determination of HRPs in plasma samples. The proposed MSPE-HPLC-UV method provided good linearity (1.5-500 ng mL-1 R2 ≥ 0.9988), low limits of detection (0.1-0.2 ng mL-1) and quantification (0.4-0.8 ng mL-1), desirable precision (RSD ≤ 8.8%, n ₌ 5), satisfactory enrichment factor (EFs ≥ 66.0), and well relative recoveries (92.8-108.8%). Overall, the established method effectively expanded the analytical potential of MSPE approach for the quantification of HRPs in biological samples.


Assuntos
Magnetismo , Água , Polissacarídeos , Adsorção , Extração em Fase Sólida/métodos , Limite de Detecção , Fenômenos Magnéticos , Cromatografia Líquida de Alta Pressão
2.
Carbohydr Polym ; 297: 119992, 2022 Dec 01.
Artigo em Inglês | MEDLINE | ID: mdl-36184161

RESUMO

In the present work, for the first time, fully green maltodextrin nanosponges (MDNSs) as extraction phases for the preparation of magnetic sorbents were introduced. All of the raw materials and synthetic methodologies used to prepare MDNSs follow the principles of green chemistry. Fluoroquinolones (FQs) (ofloxacin, ciprofloxacin, enrofloxacin, and moxifloxacin) were used as model analytes to assess the extraction performance of MDNSs in magnetic solid-phase extraction (MSPE) procedure. Under the optimized conditions, the developed MSPE was coupled with HPLC-UV to sensitively quantify trace levels of four FQs in tap water, wastewater, and river water samples. The proposed MSPE-HPLC-UV method provided wide linearity in the range of 0.25-500.0 ng mL-1 with determination coefficients ≥0.9997. Low limits of detection (LODs ≤0.06 ng mL-1) and quantification (LOQs ≤0.20 ng mL-1) were achieved. Furthermore, the developed green extraction phases compared with all other maltodextrin-based extraction phases were promising.


Assuntos
Fluoroquinolonas , Águas Residuárias , Cromatografia Líquida de Alta Pressão/métodos , Ciprofloxacina , Enrofloxacina , Fenômenos Magnéticos , Moxifloxacina , Ofloxacino , Polissacarídeos , Extração em Fase Sólida/métodos , Água
3.
Anal Bioanal Chem ; 413(30): 7609-7623, 2021 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-34668043

RESUMO

Therapeutic peptides have an important effect on physiological function and human health, so it is momentous to quantify and detect low levels of these biomolecules in biological samples for treatment and diagnostic purposes. In the present study, an efficient magnetic solid-phase extraction (MSPE) method was developed based on stearic acid-functionalized magnetic hydroxyapatite nanocomposite (MHAP/SA) as a novel and cost-effective adsorbent for extraction of five hypothalamic-related peptides (goserelin, octreotide, triptorelin, somatostatin, and cetrorelix) from biological samples. To characterize the morphology and physicochemical properties of MHAP/SA, Fourier transform infrared spectroscopy (FT-IR), energy-dispersive X-ray spectroscopy (EDS), field emission scanning microscopy (FE-SEM), CHNS elemental analysis, Brunauer-Emmett-Teller (BET), and vibrating sample magnetometry (VSM) were applied. Under optimum conditions, the proposed method (MSPE-HPLC-UV) represented favorable linearity with R2 ≥ 0.9987, suitable intra- and inter-day precisions (RSD ≤ 6.9% and RSD ≤ 8.1%, respectively, n = 3), and limits of detection and quantification in the range of 0.75-1.12 ng mL-1 and 2.50-3.75 ng mL-1, respectively. Eventually, the proposed method was used for the extraction and quantification of target therapeutic peptides in plasma and urine samples, and satisfactory relative recoveries were achieved in the range of 90.6-110.3%.


Assuntos
Durapatita/química , Hipotálamo/química , Nanocompostos/química , Peptídeos/análise , Extração em Fase Sólida/métodos , Ácidos Esteáricos/química , Cromatografia Líquida de Alta Pressão , Humanos , Limite de Detecção , Microscopia Eletrônica de Varredura , Peso Molecular , Peptídeos/sangue , Peptídeos/urina , Reprodutibilidade dos Testes , Análise Espectral/métodos
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