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1.
Analyst ; 137(17): 4076-85, 2012 Sep 07.
Artículo en Inglés | MEDLINE | ID: mdl-22785248

RESUMEN

Ionic liquids-based microwave-assisted extraction (ILs-MAE) of medicinal or useful compounds from plants was investigated as an alternative to conventional organic solvent extractions. The extraction and the preconcentration of aqueous two-phase (ATP) systems have been integrated. Various operating parameters were systematically considered by single-factor and L(9) (3(4)) orthogonal array experiments. 1-Butyl-3-methylimidazolium tetrafluoroborate ([bmim][BF(4)]) has been selected to extract Apocynum venetum. The extract was then converted to the top phase by [bmim][BF(4)]/NaH(2)PO(4) system which was suitable for the preconcentration. Reversed phase high performance liquid chromatography (RP-HPLC) with ultraviolet detection was employed for the analysis of hyperin and isoquercitrin in Apocynum venetum. The optimal experiment approach could provide higher detection limit of hyperin and isoquercitrin which were 3.82 µg L(-1) and 3.00 µg L(-1) in Apocynum venetum. The recoveries of hyperin and isoquercitrin were 97.29% (RSD = 1.02%) and 99.40% (RSD = 1.13%), respectively, from aqueous samples of Apocynum venetum by the proposed method. Moreover, the extraction mechanism of ILs-MAE and the microstructures and chemical structures of the herb before and after extraction were also investigated. The method exhibited potential applicability with other complicated samples.


Asunto(s)
Cromatografía Líquida de Alta Presión , Líquidos Iónicos/química , Microondas , Agua/química , Apocynum/química , Cromatografía de Fase Inversa , Imidazoles/química , Líquidos Iónicos/síntesis química , Medicina Tradicional China , Quercetina/análogos & derivados , Quercetina/análisis , Espectrofotometría Ultravioleta
2.
Talanta ; 116: 409-16, 2013 Nov 15.
Artículo en Inglés | MEDLINE | ID: mdl-24148423

RESUMEN

Eight kinds of green ionic liquids were synthesized, and an ionic liquid aqueous two-phase system (ILATPS) based on 1,1,3,3-tetramethylguandine acrylate (TMGA) guanidine ionic liquid was first time studied for the extraction of proteins. Single factor experiments proved that the extraction efficiency of bovine serum albumin (BSA) was influenced by the mass of IL, K2HPO4 and BSA, also related to the separation time and temperature. The optimum conditions were determined through orthogonal experiment by the five factors described above. The results showed that under the optimum conditions, the extraction efficiency could reach up to 99.6243%. The relative standard deviations (RSD) of extraction efficiencies in precision experiment, repeatability experiment and stability experiment were 0.8156% (n=5), 1.6173% (n=5) and 1.6292% (n=5), respectively. UV-vis and FT-IR spectra confirmed that there were no chemical interactions between BSA and ionic liquid in the extraction process, and the conformation of the protein was not changed after extraction. The conductivity, DLS and TEM were combined to investigate the microstructure of the top phase and the possible mechanism for the extraction. The results showed that hydrophobic interaction, hydrogen bonding interaction and the salt out effect played important roles in the transferring process, and the aggregation and embrace phenomenon was the main driving force for the separation. All these results proved that guanidine ionic liquid-based ATPSs have the potential to offer new possibility in the extraction of proteins.


Asunto(s)
Acrilatos/química , Guanidinas/química , Líquidos Iónicos/química , Microextracción en Fase Líquida/métodos , Albúmina Sérica Bovina/aislamiento & purificación , Animales , Bovinos , Análisis Factorial , Tecnología Química Verde , Enlace de Hidrógeno , Interacciones Hidrofóbicas e Hidrofílicas , Conformación Proteica , Electricidad Estática
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