RESUMEN
Ionic liquid (IL) based ultrasonic assisted extraction (ILUAE) was developed for the effective extraction of puerarin from Radix Puerariae Lobatae (RPL). The ILUAE parameters including the type of ILs, IL concentration, RPL amount, ultrasonic power and time were optimized by single-factor experiment and response surface methodology. Under the optimized experimental conditions, the best results were obtained using RPL amount 0.43 g in 10 mL 1.06 molL(-1) 1-butyl-3-methylimidazolium bromide aqueous solution, ultrasonic time 27.43 min and ultrasonic power 480 W. Scanning electron microscope images of RPL samples were obtained to provide visual evidence of the sonication effect. Compared with the conventional ultrasonic assisted extraction and refluent extraction, the proposed ILUAE offered shorter extraction time and remarkable higher efficiencies due to the higher penetration ability and solubility of IL and the cavitation phenomenon produced in the solvent by the passage of an ultrasonic wave, which further supported the suitability of the proposed approach.
Asunto(s)
Fraccionamiento Químico/métodos , Isoflavonas/aislamiento & purificación , Pueraria/química , Ultrasonido/métodos , Fraccionamiento Químico/instrumentación , Cromatografía Líquida de Alta Presión , Líquidos Iónicos , Isoflavonas/análisisRESUMEN
In this work, molecularly imprinted solid-phase extraction (MISPE) has been used to selectively enrich, purify, or remove synephrine from Aurantii Fructus Immaturus. To this end, a molecularly imprinted polymer (MIP) was prepared by self-assembly from the template synephrine, the functional monomer methacrylic acid, and the crosslinker ethylene glycol dimethacrylate in 1:4:20 molar ratio. Subsequent molecular interrogation of the MIP binding sites revealed preferential structural selectivity for synephrine relative to other structurally related naturally occurring compounds (i.e. octopamine and tyramine ). This selectivity was subsequently exploited to achieve substantial sample clean-up of extracts of crude Aurantii Fructus Immaturus and Aurantii Fructus Immaturus stir-baked with bran. The purity of synephrine in the extracts after MISPE represented approximately 24.21-fold enrichment of the synephrine in the untreated extracts of Aurantii Fructus Immaturus stir-baked with bran. High recoveries (85-90%) from the samples proved that the method was valid for selective enrichment, purification, or removal of synephrine from Aurantii Fructus Immaturus.