Green and reusable pipette tip-solid phase microextraction for the simultaneous determination of butylated hydroxyanisole, butylated hydroxytoluene, and tert-butylhydroquinone in complex food matrices by RPLC-UV

A new environmentally friendly method was developed for extracting butylated hydroxyanisole (BHA), butylated hydroxytoluene (BHT), and tert-butylhydroquinone (TBHQ) from food samples, followed by analysis using RPLC-UV. Therefore, the conditions of the pipette tip-solid phase microextraction (PT-SPE) were optimized to enhance the selectivity and extraction efficiency of these synthetic antioxidants. The proposed methodology has a linear range of 0.90–18.0 mg L −1 for BHA, 1.10–22.0 mg L −1 for BHT, and 0.83–16.6 mg L −1 for TBHQ, with repeatability of less than 4.50% and reproducibility of less than 4.00%, and good detection limits (0.047, 0.036, and 0.084 mg L −1 for TBHQ, BHA, and BHT, respectively). Optimizing the PT-SPE conditions with sample treatment enabled the application to different food samples, reduced the use of organic solvents (approximately 1.9 mL of acetonitrile), eliminated highly toxic solvents like hexane, avoided organic solvent evaporation, and was conducted without sequential step extractions. This method application enabled the precise determination of BHA, BHT, and TBHQ in oil, margarine, mayonnaise, and ketchup, with recoveries ranging from 71.95 to 113.92% and precision between 4.25 and 6.00%. Therefore, this methodology demonstrated good applicability and was eco-friendly, as indicated by the BAGI (75), AGREEprep (0.57), and Analytical Ecoscale (91) metrics, as well as the reuse of the same solid phase of PT-SPE for up to 81 extraction cycles. • Microextraction of antioxidants following Green Analytical Chemistry principles. • The same PT-SPE sorbent used for up to 81 extraction cycles with accuracy or precision. • Development of a new solid microextraction to determine synthetic antioxidants. • Miniaturized method PT-SPE-RPLC/UV determines BHA, BHT, and TBHQ in food samples. • Proposed method used in mayonnaise, oil, ketchup, and margarine without employing hexane.