| Summary: | A simple, effective, and highly sensitive analytical approach was created and applied in this study for the accurate measurement of three β<sub>2</sub>-agonist residues (clenbuterol, salbutamol, and ractopamine) in meat samples. In the course of the experiment, new adsorbent molecular sieves (ZMS)@nitrogen-doped carbon quantum dots (N-CQDs) composite materials were synthesized with the aid of hydrothermal synthesis. The composite adsorbent materials were prepared and characterized through scanning electron microscopy, transmission electron microscope, X-ray photoelectron spectroscopy, fluorescence, and zeta potential. Four determinants affecting the extraction and elution’s efficiency, such as the amount of adsorbent, the extraction time, desorption time, and the amount of extraction salt, were substantially optimized. The analytes were quantified by gas chromatography–mass spectrometry. Final results of the methodological validation reflected that the ZMS@N-CQDs composite materials were able to adsorb three β<sub>2</sub>-agonist residues well and had good reproducibility. In the meantime, all analytes indicated good linearity with coefficient of determination R<sup>2</sup> ≥ 0.9908. The limit of detection was 0.7–2.0 ng·g<sup>−1</sup>, the limit of quantification varied from 2.4 to 5.0 ng·g<sup>−1</sup>, the precision was lower than 11.9%, and the spiked recoveries were in the range of 79.5–97.8%. To sum up, the proposed approach was quite effective, reliable, and convenient for the simultaneous analysis of multiple β<sub>2</sub>-agonist residues. Consequently, this kind of approach was successfully applied for the analysis of such compounds in meat samples.
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