Coupling micro-flow liquid chromatography with Q-Orbitrap high-resolution mass spectrometry for greener, comprehensive pesticide residue analysis in fruits and vegetables

A micro-flow liquid chromatography coupled with Q-Orbitrap high-resolution mass spectrometry (micro-flow LC-HRMS) method was developed for multiresidue pesticide analysis in fruits and vegetables. The data acquisition workflow integrated full scan, variable data-independent acquisition and data-dependent MS 2 experiments. Using a 0.3 mm internal diameter column at 15 μL·min −1 , the micro-flow LC configuration enhanced ionisation efficiency and improved sensitivity, achieving instrumental limits of quantification at or below 0.010 mg·kg −1 for 239 pesticides in tomato, orange and avocado. The method showed excellent retention time and peak area stability, broad linearity, and low matrix effects for most compounds. Proficiency test and real sample results confirming its accuracy and suitability for routine monitoring. Micro-flow LC-HRMS provides a robust, sensitive and information-rich platform for pesticide residue monitoring in food, enabling comprehensive targeted quantification and non-targeted data collection within a single run. This greener approach reduces solvent consumption and waste by 25-fold compared with classical LC solutions. • Assessment of micro-flow LC-HRMS for multiresidue pesticide analysis. • Combined full scan, vDIA and ddMS 2 in a single streamlined acquisition workflow. • Achieved LOQs ≤0.010 mg·kg −1 for 239 pesticides in fruit and vegetable matrices. • Micro-flow LC-HRMS enables greener pesticide residue analysis. • Reduced solvent use by 25-fold compared with analytical-flow LC system.