A novel H3PW12O40@CS composite was prepared for the first time and utilized as a sorbent in the hollow fiber-solid phase microextraction (HF-SPME) method for the extraction of deltamethrin and cypermethrin (as a class of synthetic insecticides) from real samples using HPLC-UV. The presence of oxygen functional groups on the H3PW12O40, enhanced the interactions with selected analytes. The synergistic effect between H3PW12O40 as a sorbent and CS as a substrate with high-surface area significantly increased the extraction efficiency. The proposed method, can offer simultaneous extraction, purification and preconcentration in one step. Regarding, the clean-up ability of HF, only initial dilution with water is required before the extraction process. Also, the figures of merit were calculated at optimal conditions. Based on the results, linear dynamic range was 5×10-4 – 0.5 µg mL-1 while, the R2 exceeded 0.9927. Also, limits of detection (LODs) and limits of quantification (LOQs) were 1.9×10-4 – 2.1×10-4 µg mL-1, and 5.7×10-4 – 6.3×10-4 µg mL-1, respectively. The inter-day and intra-day relative standard deviation (RSD%) were calculated in the concentration of 5×10-4, 5×10-3 and 5×10-2 µg mL-1, which ranged in 3.40% - 5.80%. Finally, HF-SPME method was used for determination of target analytes in celery, cabbage and zucchini juices. Therefore, prepared method has advantages such as an inexpensive, simple and environmentally friendly synthesis, fast operation, low LOD and wide linear dynamic range.
