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• Amino-containing MOFs MIL-125-NH 2 was designed as a new sorbent in d-SPE. • MIL-125-NH 2 enrich the target analytes directly to improve sensitivity. • Amino-containing MIL-125-NH 2 has good adsorption capacity. • The detection limits were lower than most of traditional methods. • MIL-125-NH 2 is recovered easily and reused at least 8 times. A simple, environmentally-friendly and reliable method was developed to simultaneously monitor the residue of methyl 1-naphthalene acetate, parathion-methyl, fenitrothion, bromophos and phenthoate in pomelo by using dispersive solid-phase extraction technique (d-SPE). In this method, these target analytes were captured by MIL-125-NH 2 and detected by GC–MS/MS. The key parameters of d-SPE were optimized by the single factor experiment. Under the optimized conditions, a good determination coefficient (R2 > 0.9922) and extraction recoveries (64.7–116.8%) are obtained. The limit of detections (0.03–1.07 ng/g) is lower than the MRLs in citrus fruits established by EU (10–15000 ng/g) and China (10–10000 ng/g). The precisions of intra-day and inter-day are 1.3–8.9% and 3.8–14.9%, respectively. In addition, the sorbent MIL-125-NH 2 is stable and can be reused at least eight times. These results prove the established method is efficient and reliable to detect the pesticide residues in pomelo. [ABSTRACT FROM AUTHOR]