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An online field-assisted micro-solid-phase extraction device coupled with high-performance liquid chromatography for the direct analysis of solid samples

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Abstract

Herein, a total online device based on field-assisted extraction (FAE), micro-solid-phase extraction (μ-SPE), and high-performance liquid chromatography (HPLC) was designed. Solid samples were pretreated with ultrasound-microwave synergic effects, and then the extract was cleaned up online with a monolithic column, followed by HPLC analysis. The cross-actions between ultrasound and microwave along with other extraction parameters were studied systematically. The efficiency of this online method was verified in the determination of polycyclic aromatic hydrocarbons (PAHs) in foods and tetracycline antibiotics (TCAs) in cosmetic samples. The detection limits of nine PAHs including fluorene, phenanthrene, anthracene, fluoranthene, benzo[k]fluoranthene, benz[a]anthracene, benzo[b]fluoranthene, pyrene, and benzo[a]pyrene were all within 0.075–0.30 μg/kg, as well as four TCAs including oxytetracycline, tetracycline, chlortetracycline, and doxycycline were within 0.02–0.06 μg/kg. Six PAHs were found in roast potatoes and baked fish and the recoveries were in the range of 71.5–119.7% with RSDs of 0.2–10.9% (n = 3). The recoveries for TCAs in cosmetic samples were in the range of 75.3–118.0% with RSDs lower than 8.2% (n = 3). Compared with those offline methods, this total online FAE-μ-SPE-HPLC method not only simplifies the operation process, but also increases the precision and accuracy. Beyond trace analytes analysis in solid and semi-solid matrixes, application of this total online analysis method can also be extended to investigate field-assisted extraction mechanisms.

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Funding

This work was supported by the National Natural Science Foundation of China (nos. 21675179, 21675178, 21874159, and 21804147), the Special Funds for Public Welfare Research and Capacity Building in Guangdong Province of China (no. 2015A030401036), and the Guangzhou Science and Technology Program of China (no. 201604020165).

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  1. Ling Xia and Yuanyuan He contributed equally to this work.

Authors and Affiliations

  1. School of Chemistry, Sun Yat-sen University, Guangzhou, 510275, Guangdong, China

    Ling Xia, Yuanyuan He, Xiaohua Xiao & Gongke Li

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  1. Ling Xia
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  2. Yuanyuan He
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  3. Xiaohua Xiao
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Correspondence to Xiaohua Xiao or Gongke Li.

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Published in the topical collection New Insights into Analytical Science in China with guest editors Lihua Zhang, Hua Cui, and Qiankun Zhuang.

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Xia, L., He, Y., Xiao, X. et al. An online field-assisted micro-solid-phase extraction device coupled with high-performance liquid chromatography for the direct analysis of solid samples. Anal Bioanal Chem 411, 4073–4084 (2019). https://doi.org/10.1007/s00216-019-01809-y

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  • DOI: https://doi.org/10.1007/s00216-019-01809-y

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