Determination of low-concentration pesticides in real samples requires a simple, rapid, low-solvent-consumption, and high-efficiency extraction method before introduction into the chromatography system. In the present research, the objectives mentioned were achieved by using the developed NH2-MIL-101(Cr)/SBA-15 nano composite with high extraction efficiency as a sorbent in the syringe filter–solid-phase extraction (SPE) approach, which is easy to use and has low solvent consumption. In this study, for the first time, the metal–organic framework NH2-MIL-101(Cr) was combined with Santa Barbara Amorphous-15 (SBA-15) and was used as sor bent in syringe filter-SPE for extracting some pesticides from environmental water samples. To verify the suc cessful formation of the nanocomposite, several characterization techniques including SEM, FTIR, XRD, TGA, and BET were employed. Furthermore, the variables affecting the extraction efficiency of NH2-MIL-101(Cr)/SBA- syringe - filter-SPE-HPLC, such as the sample volume, pH, volume of eluting solvent, and type of eluting sol vent were optimized by utilizing a response surface methodology (RSM) based on central composite design (CCD). The results demonstrated that the NH₂-MIL-101(Cr)/SBA-15 composite exhibited superior adsorption performance and lower detection limits for the target pesticides compared to the unmodified NH₂-MIL-101(Cr). The method achieved detection limits ranging from 0.07 to 0.6 μ 800.0 μ g/L, with a linear response range of 0.25 to g/L. It also showed strong repeatability, with relative standard deviation (RSD) values between 2.8 % and 5.0 %, and excellent recovery rates of 90 % to 105 % at spiked concentrations from 2.0 to 40.0 μ g/L.
