Conveniently monitoring aldehyde changes in heated edible oils using miniaturized kapok fiber-supported liquid-phase extraction/in-situ derivatization coupled with liquid chromatography-tandem mass spectrometry.

[Display omitted] • Mini-KF-SLE-ISD was developed for aldehyde sample preparation in edible oil. • Simultaneous derivatization and extraction of aldehydes in edible oils were achieved. • Box-Behnken design optimization resulted in enhanced detection sensitivity. • The method proved simple, cost-effective, highly sensitive, and easy to automate. • Aldehyde changes during heating exhibited distinctions among various oil types. Heating edible oils generates aldehydes, potentially leading to adverse health effects, making their analysis essential for quality control. This study presents a convenient miniaturized kapok fiber-supported liquid-phase extraction/ in-situ derivatization method for the simultaneous extraction and derivatization of aldehydes in oils. The method involves placing 150 mg oil into a 1 mL pipette tip packed with 25 mg kapok fiber, adding 150 μL ACN with 1.5 mg mL−1 DNPH, and post 30-minute static extraction, retrieving the extractant with a pipettor for liquid chromatography-tandem mass spectrometry analysis. By optimizing critical parameters through a Box-Behnken design, the method exhibits good linearity (1–500 ng g−1, R2 ≥ 0.991), low detection limits (0.2–1.0 ng g−1), excellent accuracy (95.3–107.1%) and high precisions (relative standard deviation < 7.9%). This method simplifies sample preparation processes, cuts solvent use, and facilitates automation. It effectively identifies ten aldehyde variations in six heated oils, displaying distinct profiles consistent with prior research. [ABSTRACT FROM AUTHOR]