Development of a silica monolith modified with Fe₃O₄ nano‐particles in centrifugal spin column format for the extraction of phosphorylated compounds

Abstract

In this study, citrate-stabilised iron oxide nano-particles (∼16 nm) have been immobilised on commercial silica monolithic centrifugal spin columns (MonoSpin) for the extraction of phosphorylated compounds. Two alternative strategies were adopted involving either direct electrostatic attachment to an aminated MonoSpin (single-layer method) in the first instance, or the use of a layer-by-layer method with poly(diallyldimethylammonium) chloride. Field-emission scanning electron spectroscopy and energy-dispersive X-ray spectroscopy was used for confirming notably higher coverage of nano-particles using the layer-by-layer method (2.49 ± 0.53 wt%) compared with the single-layer method (0.43 ± 0.30 wt%). The modified monolith was used for the selective separation/extraction of adenosine monophosphate, adenosine diphosphate and adenosine triphosphate with elution using a phosphate buffer. A reversed-phase liquid chromatographic assay was used for confirming that adenosine, as a non-phosphorylated control was not retained on the modified MonoSpin devices, whereas recovery of 80% for adenosine monophosphate, 86% for adenosine diphosphate and 82% for adenosine triphosphate was achieved.

Trace determination of antifungal drugs in biological fluids through a developed approach of hydrogel‐based spin‐column micro‐solid‐phase extraction followed by LC‐MS/MS analysis

“…Recently, some literature deals with applying spin-column micro-SPE (SC-μSPE) as an attractive sample preparation method for analyzing target analytes in biological and environmental matrices [12,13]. In this case, a small amount of sorbent is packed into a column, and loading of sample, washing, and elution procedures are executed by centrifugation as a gravitational force to accomplish the process [14,15]. Controlling the passing flow rate is carried out by constant centrifugation speed to ensure reproducibility, and subsequently, the method precision would be enhanced thanks to the usage of a centrifuge with a programmable speed [12,13].…”

“…Controlling the passing flow rate is carried out by constant centrifugation speed to ensure reproducibility, and subsequently, the method precision would be enhanced thanks to the usage of a centrifuge with a programmable speed [12,13]. Moreover, SC-μSPE has other unique advantages such as simple operation procedure, rapidity, requiring low elution volume, and not involving solvent evaporation [12,[14][15][16]. The prerequisite for efficient sample pretreatment depends on the proper choice of the sorbent in SC-μSPE.…”

Histidine-modified organic-silica hybrid monolithic column for mixed-mode per aqueous and ion-exchange capillary electrochromatography

“…According to the nature of matrix chemistry, monolithic columns can be mainly classified into organic polymer-based [8][9][10][11], inorganic silica-based [12][13][14], and organic-silica hybrid monolithic columns [15][16][17][18][19][20][21][22][23]. Organic polymer-based monolithic columns show good stability toward pH changes and their surfaces can be easily tuned by using a variety of functional monomers and cross linkers.…”

“…In recent years, monoliths, which can be described as integrated continuous porous separation media for separation science, have become well‐established stationary phases in the field of CEC due to the simplicity of their in situ preparation method, ready control of their porous properties and surface chemistries as well as their unique structure and exceptional characteristics . According to the nature of matrix chemistry, monolithic columns can be mainly classified into organic polymer‐based , inorganic silica‐based , and organic‐silica hybrid monolithic columns . Organic polymer‐based monolithic columns show good stability toward pH changes and their surfaces can be easily tuned by using a variety of functional monomers and cross linkers.…”

Selective separation and determination of the synthetic colorants in beverages by magnetic solid-phase dispersion extraction based on a Fe3O4/reduced graphene oxide nanocomposite followed by high-performance liquid chromatography with diode array detectio

“…For example, 2‐D planar graphene sheets were immobilized onto silica‐coated magnetic microspheres by simple adsorption, and the graphene sheets were used as adsorbent material to extract six sulfonamide antibiotics (SAs) from water samples . The nanocomposite of Fe 3 O 4 and reduced graphene oxide (Fe 3 O 4 /rGO) possessed superior stability and biocompatibility, and was introduced into many studies due to the high extraction capacity of graphene and fast separation of superparamagnetic Fe 3 O 4 .…”