Successive pH- and heat-induced homogenous liquid–liquid extraction

• For the first time, successive pH- and heat-induced HLLE has been developed.
• The method is applied in analysis of pesticides in fruit juices and vegetables.
• LODs are achievable at ng g−1 using HPLC-DAD.
• The method has high EFs and ERs, low LODs, and short extraction time.

A simple and efficient analytical method known as pH- and heat-induced homogenous liquid-liquid extraction combined with high-performance liquid chromatography has been successfully developed for the extraction and determination of neonicotinoid pesticides in aqueous samples. In this method, a few mL of a water-miscible basic extraction solvent is mixed with a high volume of an aqueous phase containing the analytes and passed through a tube which a portion of the tube is filled with sodium carbonate as a separating agent. By passing the solution, salt is dissolved and the fine droplets of the extraction solvent are formed. The produced droplets go up through the remained solution and collect as a separated layer. In the following, the collected organic phase is removed and placed into a micro tube. Then it is heated in a water bath to form two phases. Several experimental parameters that influence extraction efficiency such as type and volume of extraction solvent, type of phase separation agent, temperature, and extraction time were investigated. Under the optimum conditions, the extraction recoveries and enrichment factors ranged between 51 and 81% and 680 and 1080, respectively. Calibration curves showed a high-level of linearity for all target analytes with coefficients of determination ranging between 0.997 and 0.999. The repeatability of the proposed method expressed as relative standard deviation varied between 3 and 5% (n = 6, C = 50 μg L−1), and the detection limits were in the range of 0.52–1.0 μg L−1. Finally, the performance of the method was evaluated by analyzing the selected pesticides in different fruit juice and vegetable samples.