RESUMEN
The novel molecularly imprinted microspheres for four phenylarsonic compounds have been firstly prepared with the reversible addition-fragmentation chain transfer polymerization in a suspension system. The resulting polymeric microspheres were characterized by infrared spectrum, scanning electron microscope and differential scanning calorimetry. With serial adsorption experiments, the polymeric microspheres showed highly specific molecular recognition, fast mass transfer rate and robust adsorption of the substrates. Then, the imprinted polymer was used as the solid-phase extraction adsorbent to extract the phenylarsonic compounds from the feeds, edible chicken and pork. The cartridge was washed with 2 mL ethyl acetate and eluted with 3 mL of methanol- acetic acid (90:10, v/v). The recoveries of the molecularly imprinted solid-phase extraction (MISPE) column ranged from 83.4% to 95.1%. This work provided a versatile approach for the specific extraction of the organoarsenic compounds from complicated matrices and exhibited a bright future for the application of MISPE column.
Asunto(s)
Alimentación Animal/análisis , Arsenicales/análisis , Carne/análisis , Impresión Molecular , Polímeros/química , Extracción en Fase Sólida/métodos , Adsorción , Animales , Ácido Arsanílico/análogos & derivados , Ácido Arsanílico/análisis , Ácido Arsanílico/aislamiento & purificación , Arsenicales/aislamiento & purificación , Pollos , Cromatografía Líquida de Alta Presión , Músculos/química , Roxarsona/análisis , Roxarsona/aislamiento & purificación , PorcinosRESUMEN
To study the separation of p-aminobenzenearsonic acid (PABAA) and its oxide, p-aminophenylarsine oxide (PAPAO), both the absorption spectra were scanned at the wavelengths from 200 nm to 380 nm. PABAA had absorption maximum at 254 nm and PAPAO 258 nm. The effects of salt concentration, column temperature, methanol and ion-pair agent concentrations on the capacity factor were investigated. Compounds of high polarity showed almost no retention on reversed-phase column; as the volume fraction of the methanol decreased from 90% to 10%, the retention time of PABAA gradually increased with broad peak, and partially eluted when methanol volume fraction being below 20%. With temperature rising, the retention time of PABAA was decreased. But PABAA capacity factor can be increased by selecting an appropriate salt concentration for the mobile phase. The cetyltrimethyl and tetrabutyl ammonium ions were separately added as ion-pair agents to the mobile phase containing methanol in phosphate buffer of 10 mmol/L, the changes of retention time were observed. The mechanism of retention based on reversed phase ion-pair model is proposed. Besides, the retention behaviour is also influenced by size exclusion in stationary phase as well as polar interactions with residual silanol group on the silica surface.