A method was developed to determine 20 illegal residual -agonists in pork tissues, including muscle and liver simultaneously. The samples were hydrolyzed by -glucuronidase, purified by PCX SPE cartridges, and detected by HPLC coupled with electrospray ionization MS/MS operating in the positive ion mode. Matrix-fortified calibration was performed to compensate for the matrix effect and loss in sample preparation. Decision limit ranged from 0.05 to 0.23 g/kg in muscle and 0.05 to 0.57 g/kg in liver. Decision capacity ranged from 0.11 to 0.4 g/kg in muscle and 0.16 to 0.79 g/kg in liver. In Food Analysis Performance Assessment Scheme proficiency test 0287, a pig liver test material containing 13 -agonists was analyzed using the method developed, and clenbuterol and ractopaime were confirmed as being present. Z-scores for clenbuterol and ractopaime were 0.2 and 0.6, respectively.
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