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Determination Of Glucocorticoids Residues In Animal Derived Food And Urine By Ultra Performance Liquid Chromatography-Electrospray Tandem Mass Spectrometry

Posted on:2007-02-23Degree:DoctorType:Dissertation
Country:ChinaCandidate:X L CuiFull Text:PDF
GTID:1101360212470806Subject:Applied Chemistry
Abstract/Summary:PDF Full Text Request
As the fast development of economy, animal derived food is becoming more and more important in our life, but hormone residues in every kind of animal derived food has become a hot topic of public health. In this paper, a comprehensive analytical method based on ultra performance liquid chromatography-electrospray tandem mass spectrometry (UPLC-MS/MS) with negative mode has been developed for the simultaneous determination of glucocorticoids residues in animal derived food and urine. Multi-reaction monitoring mode was employed for the determination. Samples were extracted with methanol after the buffer solution was added, then defatted with n-hexane (except urine samples). Sample concentration and purification were performed using GCB and amino-propyl solid extraction cartridge. The separation was performed on a Waters ACQUITY UPLCTM BEH C18 column with a gradient system of methanol and water (containing 0.1% formic acid) as mobile phase at a flow rate of 0.3 ml/min. The qualification analysis was done by using retention time and distribution of diagnostic ion pairs, and the quantification analysis was based on the peak intensity of parent ion and a fragment ion with higher signal. The detection limits (LOD) of the method were from 0.003 to 0.38μg/kg and the limits of quantification (LOQ) ranged from 0.011 to 1.27μg/kg, average recoveries of glucocorticoids (spiked at the levels of 2, 0.4μg/kg) ranged from 81.0% to 112.3%, with relative standard deviations between 1.8% and 16.6%. Routine tests showed the method was fast, sensitive and specific for the glucocorticoids residues determination.The separation for betamethasone and dexamethasone was performed on a Waters ACQUITY UPLCTM BEH C18 column with a gradient system of acetonitrile and water (containing 0.1% formic acid) as mobile phase, and an analytical method based on UPLC-MS/MS has been developed for the simultaneous determination of betamethasone and dexamethasone residues in animal derived food and urine. The...
Keywords/Search Tags:Ultra Performance Liquid Chromatography-Electrospray Tandem Mass Spectrometry, Glucocorticoids, Animal Derived food, Residues, Solid Phase Extraction
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