One-pot preparation of magnetic composite containing boronic acid groups and aminated multwalled carbon nanotubes for the speciation of Se(IV) and Se(VI) in water and milk samples by combination with chromatographic quantification

Abstract

Speciation of Se(IV) and Se(VI) is essential due to their significant differences in reactivity, toxicity and bioavailability. Efficient extraction is the pivotal step in the quantification of inorganic selenium species. In this work, a new magnetic nano-composite (MNC) containing boronic acid group and aminated multwalled carbon nanotubes was facilely fabricated by means of one-pot hydrothermal strategy. The prepared MNC contained abundant functional groups and satisfactory magnetic saturation value. Combining with magnetic solid phase extraction (MSPE) format, the MNC displayed satisfactory capture performance towards the complex formed by the coordination of Se(IV) and o-phenylenediamine (OPA). Adsorption isotherm and adsorption kinetics were studied in detail to investigate the adsorption procedure of Se(IV)/OPA complex on MNC. Under the optimal preparation conditions of MNC and extraction parameters, the MNC/MSPE was connected with HPLC equipped with a diode array detector (DAD) to quantify trace Se(IV) and Se(VI) species in water and milk samples. Se(VI) was reduced to Se(IV) and then the total inorganic Se was quantified by the developed method. Subtraction method was used to measure the concentration of Se(VI). The achieved limits of detection were in the ranges of 0.0082–0.013 μg/L and 0.041–0.13 μg/kg for water and milk samples, respectively. Recoveries in actual samples spiked with different amounts of analytes varied from 81.0 % and 117 %, and the RSDs for repeatability varied from 1.0 % to 10 %. In comparison with existing studies based on MSPE, the established method presents some merits such as greenness in the preparation of magnetic adsorbent, rapid extraction procedure, low cost and satisfactory sensitivity in the speciation of inorganic Se species.