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

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. Graphical abstract.