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Determination of Antimony Speciation in Cow Milk Using Dispersive Micro-solid Phase Extraction Based on Fibrous TiO2@g-C3N4 Nanocomposites and ICP-MS After Sample Pretreatment by Artificial Gastric Juice

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Abstract

In this work, fibrous TiO2@g-C3N4 nanocomposites (FTGCNCs) were used as a new adsorbent of dispersive micro-solid phase extraction for speciation of antimony in cow milk, including Sb(III), Sb(V), residual, digestible, and total Sb. Samples were prepared with artificial gastric juice to achieve bioaccessible species of elements before ICP-MS determination. Besides, adsorption behaviors of Sb(III) and Sb(V) on FTGCNCs were investigated. The results showed that Sb(III) was quantitatively adsorbed on FTGCNCs in the pH range of 2.0–4.0, while Sb(V) remained in aqueous phase. Sb(III) adsorbed on FTGCNCs was eluted completely with 1.5 mol L−1 HNO3 solution. The assay of Sb(V) was based on subtracting Sb(III) from total Sb. Total Sb was extracted and determined after the reduction of Sb(V) into Sb(III). The main parameters affecting the separation and determination of the analytes were examined in detail. Under optimal conditions, the limit of detection was 0.37 pg mL−1 for Sb(III) with relative standard deviation of 4.1% (c = 1.0 ng mL−1, n = 9). This method was successfully used for the analysis of Sb speciation in cow milk. To validate this method, a certified reference material of milk powder was analyzed, and the determined values were in good agreement with the certified values.

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Funding

This work was financially supported by the Nature Science Foundation of Hubei Province (No. 2019CFB159) and the Research and Innovation Initiatives of Wuhan Polytechnic University (No. 2018J04 and 2018Y07).

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Authors and Affiliations

  1. College of Food Science and Engineering, Wuhan Polytechnic University, Wuhan, 430023, People’s Republic of China

    Shizhong Chen & Dengbo Lu

  2. College of Chemical and Environmental Engineering, Wuhan Polytechnic University, Wuhan, 430023, People’s Republic of China

    Yuxiu Liu, Chunlei Wang & Juntao Yan

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  1. Shizhong Chen
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Correspondence to Shizhong Chen.

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Shizhong Chen declares that he has no conflict of interest. Yuxiu Liu declares that he has no conflict of interest. Chunlei Wang declares that she has no conflict of interest. Juntao Yan declares that he has no conflict of interest. Dengbo Lu declares that she has no conflict of interest.

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Chen, S., Liu, Y., Wang, C. et al. Determination of Antimony Speciation in Cow Milk Using Dispersive Micro-solid Phase Extraction Based on Fibrous TiO2@g-C3N4 Nanocomposites and ICP-MS After Sample Pretreatment by Artificial Gastric Juice. Food Anal. Methods 13, 2102–2110 (2020). https://doi.org/10.1007/s12161-020-01818-z

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