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Direct immersion solid-phase microextraction (DI-SPME) coupled with gas chromatography–mass spectrometry (GC–MS) was developed for rapid analysis of clenbuterol in pork for the first time. In this work, a low-cost homemade 44 µm polydimethylsiloxane (PDMS) SPME fiber was employed to extract clenbuterol in pork. After extraction, derivatization was performed by suspending the fiber in the headspace of the 2 mL sample vial saturated with a vapor of 100 µL hexamethyldisilazane. Lastly, the fiber was directly introduced to GC–MS for analysis. All parameters that influenced absorption (extraction time), derivatization (derivatization reagent, time and temperature) and desorption (desorption time) were optimized. Under optimized conditions, the method offered a wide linear range (10–1000 ng g −1 ) and a low detection limit (3.6 ng g −1 ). Finally, the method was successfully applied in the analysis of pork from the market, and recoveries of the method for spiked pork were 97.4–105.7%. Compared with the traditional solvent extraction method, the proposed method was much cheaper and fast.

Rapid Determination of Clenbuterol in Pork by Direct Immersion Solid-Phase Microextraction Coupled with Gas Chromatography–Mass Spectrometry