期刊
JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
卷 60, 期 8, 页码 1898-1905出版社
AMER CHEMICAL SOC
DOI: 10.1021/jf2039058
关键词
beta(2)-agonists and beta-blockers; high-performance liquid chromatography; linear ion trap mass spectrometry; consecutive reaction monitoring; animal food
资金
- National Natural Science Founding of China [20837003]
- Ministry of Health [200902009]
A sensitive method has been developed for the simultaneous determination of residues of 25 beta(2)-agonists and 23 beta-blockers in animal foods by high-performance liquid chromatography coupled with linear ion trap mass spectrometry (HPLC-LIT-MS). This method is based on a new procedure of hydrolysis and extraction by 5% trichloracetic acid, and then cleaned up by mixed strong cation exchange (MCX) cartridges coupled with a novelty cleanup step by methanol. Methanol and 0.1% formic acid were used as mobile phases for gradient elution, while a Supelco Ascentis Express Rp-Amide column was used for LC separation. ESI positive ion scan mode was used with consecutive reaction monitoring (CRM, MS3). Nine beta(2)-agonists labeled by the deuterium isotope were used as internal standards for quantification. The linear ranges of 48 analytes were from 5 to 200 mu g/L; the coefficient of correlation was not less than 0.995. Blank pork muscle, blank liver, and blank kidney were selected as representative matrix for spiked standard recovery test. The recoveries of each compound were in the range of 46.6-118.9%, and the relative standard deviations were in the range of 1.9-28.2%. Decision limits (CC alpha, alpha = 0.01) of 48 analytes in muscles, liver, and kidney samples ranged from 0.05 to 0.49 mu g/kg, and the detection capability (CC beta, beta = 0.05) ranged from 0.13 to 1.64 mu g/kg. This method was successfully applied to 110 real animal origin food samples including meat, liver, and kidney of pig and chicken samples.
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