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Study On Determination Of Macrolide Antibiotics Residues In Animal Derived Food By UPLC-MS/MS

Posted on:2009-11-28Degree:MasterType:Thesis
Country:ChinaCandidate:X Y WuFull Text:PDF
GTID:2154360308478024Subject:Analytical Chemistry
Abstract/Summary:PDF Full Text Request
Macrolide antibiotics as a kind of very important antibiotics are used extensively in medicine and veterinary medicine in order to cure and prevent bacterial infection. But it derived negative consequences. The most attended problem is that obtaining of tolerance to bacteria bring risk to animal, health and environment. EU lead the world in the risk prevention of macrolide antibiotics as feed additives, in 1997 EU introduced the ban on use of SPM and TYL, until 2001 EU thoroughly ban all of dose as promoting growth. Therefore, the residue analysis of macrolide antibiotics in animal derived food is a major concern.This paper established a UPLC-MS/MS method for simultaneous determination of eight macrolide antibiotics in animal derived food, including eggs, milk and pig tissues (pork, kidney, liver). LC separation was performed on an ACQUITY UPLC BEH C18 column (100 mm×2.1 mm,1.7μm). Mobile phase was optimized as methanol and water containing 0.1% formic acid. Macrolide antibiotics were extracted from eggs and milk with ACN, as well as from pork, kidney, liver with phosphoric buffer (pH=6.0). Extracts were passed through the HLB cartridges which had been conditioned with 6.0 mL methanol and 6.0 mL water. After being rinsed with 10.0 mL water: methanol (8:2), The analytes were eluted with 6.0 mL methanol. The linear range of calibration curves were 0.2 to 100.0μg/kg for all the analytes with acceptable R2>0.9709. The recoveries, of eight macrolide antibiotics at fortified levels of 0.5,1.0,5.0μg/kg ranged from 74.0 to 125.5%, RSD ranged from 2.4 to 24%. LOD were in the range of 0.07~0.1μg/kg, LOQ 0.2-0.4μg/kg.The research results indicate that the whole method is accurate and sensitive.
Keywords/Search Tags:Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry, Macrolide antibiotics, Solid Phase Extraction, Animal Derived Food
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