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Synthesis of SiO2@MOF-199 as a Fiber Coating for Headspace Solid-Phase Microextraction of Phthalates in Plastic Bottled Milk

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Abstract

In this paper, SiO2@MOF-199 composite with core–shell structure was prepared by in-situ growth of MOF-199 on the surface of SiO2 microspheres, and SiO2@MOF-199 coated fiber was prepared for headspace solid phase microextraction (HS-SPME) of phthalate esters (PAEs) in plastic bottled milk. The prepared SiO2@MOF-199 has both mesoporous structure of SiO2 and microporous structure of MOF-199. The hierarchical porous structure not only gives the analyte higher adsorption performance, but also improves the diffusion rate of the analyte in SiO2@MOF-199. The coated fibers have good thermal stability and are relatively uniform in size and structure. The extraction conditions of the prepared fibers for PAEs were optimized by single factor optimization and response surface Box-Behnken design. Under optimized conditions, the fiber displays wide linear ranges of PAEs (dimethyl phthalate, diethyl phthalate and diallyl phthalate are 5–800 ng L−1, di-n-butyl phthalate, butyl benzyl phthalate and di-n-octyl phthalate are 50–1000 ng L−1), low limits of detection (0.3–19.8 ng L−1), and high enrichment factors (325–2089). The intra-day and inter-day relative standard deviations (RSD) for PAEs extractions using a single fiber were (4.7–8.5%) and (5.7–9.1%), respectively. The fiber-to-fiber reproducibility for three fibers prepared in parallel was 7.2–11.3% (RSD). The method was successfully applied to the extraction of PAEs from plastic bottled milk and to the quantitation by a gas chromatograph with a flame ionization detector. The average recoveries were 84.0% to 105%.

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Acknowledgements

This work was supported by the Natural Science Foundation of Hebei Province (B2016201213, B2016201210), Research Innovation Team of College of Chemistry and Environmental Science of Hebei University (hxkytd-py2101) and Hebei University Student' Innovation and Entrepreneurship Training Program of China (2021187).

Funding

Natural Science Foundation of Hebei Province,B2016201213,Yun-Kai Lv,B2016201210,Li-Qing Yu,Research Innovation Team of College of Chemistry and Environmental Science of Hebei University,hxkytd-py2101,Yun-Kai Lv,Hebei University Student' Innovation and Entrepreneurship Training Program of China,2021187,Zhao Yang

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  1. Key Laboratory of Analytical Science and Technology of Hebei Province, Key Laboratory of Medicinal Chemistry and Molecular Diagnosis of Ministry of Education, College of Chemistry and Environmental Science, Hebei University, 180 Wusi East Road, Baoding, 071002, China

    Xiao-Xue Jiang, Yue-Na Sun, Chen Zhang, Zhao Yang, Li-Qing Yu & Yun-Kai Lv

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  1. Xiao-Xue Jiang
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Correspondence to Yue-Na Sun or Yun-Kai Lv.

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Jiang, XX., Sun, YN., Zhang, C. et al. Synthesis of SiO2@MOF-199 as a Fiber Coating for Headspace Solid-Phase Microextraction of Phthalates in Plastic Bottled Milk. Chromatographia 85, 851–863 (2022). https://doi.org/10.1007/s10337-022-04184-6

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