Enantioselective Determination of Chiral Fungicides in Food Samples Using Automated Dispersive Microextraction Coupled With UHPLC–MS/MS

ABSTRACT An enantioselective analytical method based on automated dispersive liquid–liquid microextraction (DLLME) and ultrahigh‐performance liquid chromatography coupled with tandem mass spectrometry (UHPLC–MS/MS) was developed for the detection of chiral triazole fungicides (TFs) in food samples. Fatty acids were used as extractants and bio‐derived solvents as dispersants, thereby eliminating the need for toxic reagents. An eight‐channel automated pipetting workstation with deep‐hole plates precisely dispensed four batches of extractant (octanoic acid) and dispersant (γ‐valerolactone) into four sample sets simultaneously, enhancing sample throughput and pipetting accuracy while minimizing manual errors. Using sodium chloride solution as a demulsifier allowed rapid phase separation within a short time, eliminating the need for traditional centrifugation. The DLLME–UHPLC–MS/MS method indicated good linearity in the concentration range of 0.05–5 µg L −1 with the limits of detection and quantification of 0.015 and 0.05 µg L −1 , respectively. This method was successfully applied to water, juice, wine, and tea, yielding recoveries ranging from 70.3% to 101.8%. It achieved good enrichment efficiency with a pre‐concentration factor range of 29.3–42.4. The automated sample pretreatment strategy developed in this study offers an efficient, accurate, and environment‐friendly approach for analyzing chiral fungicide residues in food matrices.