期刊
JOURNAL OF SEPARATION SCIENCE
卷 33, 期 1, 页码 1-10出版社
WILEY-V C H VERLAG GMBH
DOI: 10.1002/jssc.200900314
关键词
Food analysis; IT; LC-MS; Pesticides; Pressurized liquid extraction
资金
- Spanish Ministry of Education and Science
- European Regional Development Funds (ERDF) [GCL2007-66687-C02-01]
- Conselleria de Sanitat of the Generalitat valenciana [PLAT2008-A-004]
A method based on pressurized liquid extraction and LC-MS/MS has been developed for determining nine benzoylureas (BUs) in fruit, vegetable, cereals, and animal products. Samples (5 g) were homogenized with diatomaceous earth and extracted in a 22 mL cell with 22 mL of ethyl acetate at 80 degrees C and 1500 psi. After solvent concentration and exchange to methanol, BUs were analyzed by LC-MS/MS using an IT mass analyzer, which achieved several transitions of precursor ions that increase selectivity providing identification. LOQs were between 0.002 and 0.01 mg/kg, which are equal or lower than maximum residue limits established by the Codex Alimentarius. Excellent linearity was achieved over a range of concentrations from 0.01 to 1 mg/kg with correlation coefficients 0.995-0.999 (n = 7). Validation of the total method was performed by analyzing in quintuplicate seven different commodities (milk, eggs, meat, rice, lettuce, avocado, and lemon) at three concentration levels (0.01, 0.1, and 1 mg/kg). The recoveries ranged from 58 to 97% and the RSDs from 5 to 19% depending on the compound and the commodity. The combination of pressurized liquid extraction with LC-MS/MS provides a sensitive and selective method for the determination of BUs in food.
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