期刊
JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
卷 60, 期 44, 页码 11005-11014出版社
AMER CHEMICAL SOC
DOI: 10.1021/jf303222a
关键词
Fluoroquinolones; LC-MS/MS; triple quadrupole; molecularly imprinted polymers; solvent extraction; solid-phase extraction; eggs; wildlife eggs
资金
- Spanish Ministry of Science and Innovation (SCARCE) [CSD-665-2009]
- Spanish Ministry of Science and Innovation [CGL2011-29703-C02-02]
A sensitive, selective, and efficient method was developed for simultaneous determination of 11 fluoroquinolones (FQs), ciprofloxacin, danofloxacin, difloxacin, enrofloxacin, flumequine, marbofloxacin, norfloxacin, ofloxacin, oxolinic acid, pipemidic acid, and sarafloxacin, in eggs by molecularly imprinted polymer (MIP) and column liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS). Samples were diluted with 50 mM sodium dihydrogen phosphate at pH 7.4, followed by purification with a commercial MIP (SupelMIP SPE-Fluoroquinolones). Recoveries for the 11 quinolones were in the range of 90-106% with intra- and interday relative standard deviation ranging from 1 to 6% and from 3 to 8%, respectively. Limits of detection (LODs) were 0.12-0.85 ng/g, and limits of quantification (LOQs) were 036 and 239 ng/g, whereas the decision limit (CC alpha) and detection capability (CC beta) ranged from 0.46 to 3.35 ng/g and from 0.59 to 4.12 ng/g, respectively The calculated relevant validation parameters are in an acceptable range and in compliance with the requirements of Commission Decision 2002/657/EC. Moreover, a comparison to two other sample treatments [solid phase extraction (SPE) and solvent extraction] has been carried out The method was applied to lying hens, Japanese quail, and black headed gull eggs, in which FQs were not found. The method was also applied to study the depletion of sarafloxacin in eggs.
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