Rapid analysis of triazine herbicides in fruit juices using evaporation-assisted dispersive liquid–liquid microextraction with solidification of floating organic droplets and HPLC-DAD

Abstract

A rapid and convenient analytical procedure (evaporation-assisted dispersive liquid–liquid microextraction with solidification of floating organic droplets) is advanced for determining the concentrations of triazine herbicide residues (e.g. simazine and atrazine) in fruit juices via HPLC-DAD. The technique involves adding 1-dodecanol (low density) and dichloromethane (high density) to the test solution to act as the extraction and volatile solvents, respectively. Calcium oxide is added to generate heat to accelerate the evaporation of dichloromethane, whereupon the 1-dodecanol quickly disperses into small droplets to complete the microextraction process. Thus, there is no need to use a dispersive solvent and heating equipment is also not required. The floating 1-dodecanol is subsequently frozen using an ice bath to facilitate its separation from the sample. Under optimal conditions (250 μL of 1-dodecanol (extraction solvent), 150 μL of CH₂Cl₂ (volatile solvent), 1250 mg of CaO, and an extraction time of 60 s) the detection procedure is linear over the range 0.05–5 μg mL⁻¹ (with R > 0.99). The limits of detection (LOD) and quantification (LOQ) were determined to be 0.0022–0.0034 μg mL⁻¹ and 0.0073–0.0113 μg mL⁻¹, respectively. The recovery of simazine and atrazine in three fruit juices ranged between 78.5% and 96.4% with a relative standard deviation <8.2%. Therefore, the proposed approach can be effectively adopted to analyze the triazine herbicide content in fruit juices. The method has been proved to be simple, reliable, and remarkably efficient.