Triazole compounds have been globally used for controlling fungal diseases such as rusts, powdery mildew, and many leaf-spotting fungi. These compounds also have adverse effects on the environment and human health. In the present work, a hydrogel-based sorbent was synthesized by a combination of hydrophilic acrylic polymer and biodegradable amylodextrin. The sorbent was characterized by Fourier-transform infrared (FT-IR) spectroscopy, Brunauer-Emmett-Teller (BET) surface area, elemental CHN analysis, field emission scanning electron micro-scopy (FE-SEM), and zeta potential. The synthesized hydrogel was used as a green sorbent in the pipette-tip micro-solid phase extraction procedure for extraction and quantification of triazole fungicides (penconazole, hexaconazole, and tebuconazole) in environmental water samples. The corona discharge-ion mobility spec-trometry (CD-IMS) was used as a rapid and sensitive detection technique. The effects of important variables on the extraction efficiency were optimized by response surface methodology (RSM). The proposed method pro-vided good linearity (r2 & GE; 0.995) over a concentration range of 0.5-1000 ng/mL, acceptable intra-day RSD (& LE; 5.7%, n = 5) and inter-day RSD (& LE; 8.7%, n = 5), low limits of detection (0.10-0.20 ng/mL), good preconcen-tration factors (16.9-17.9 times), and high extraction recoveries (93.1-98.3%) under optimum extraction con-ditions. The extraction conditions were as follows: the amount of sorbent: 6.0 mg, pH of sample solution: 7.5, the flow rate of sample solution: 2.0 mL/min, adsorption time: 16.5 min, volume of desorption solvent: 1.1 mL, the flow rate of desorption solvent: 0.5 mL/min, and desorption time: 11.7 min. Finally, the proposed method was successfully applied for the quantification of triazoles in river and agricultural water samples.