A solid-phase extraction (SPE) sorbent, a Zn(II) based metal–organic framework, was prepared via a simple, solventless, green and a low-cost mechanosynthesis process. This sorbent was applied to the extraction of three plasticizer compounds (Di-n-butyl phthalate (DBP), di-2-(ethylhexyl) phthalate (DEHP) and dioctyladipate (DOA)) prior to analysis by gas chromatography with a flame ionization detector (GC-FID). The applied sorbent had the advantages of large surface area, simple and low cost preparation process and good stability. Analytical performances of the proposed method were investigated under the optimum extraction conditions and compared with other SPE methods reported for the same analytes. Validation experiments showed that the optimized method presents good linearity (R2 > 0.994), satisfactory precision (RSD ≤ 6.3%), and suitable pre-concentration factors (92–295). The results indicated that solid phase extraction with the proposed sorbent had advantages of convenience, good sensitivity, high efficiency, and it could also be applied successfully to analyze plasticizers in real water samples.
