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Determination Of Antifungal Drug Residues In Food

Posted on:2011-09-14Degree:MasterType:Thesis
Country:ChinaCandidate:Y YuFull Text:PDF
GTID:2144360305484925Subject:Chemical Engineering and Technology
Abstract/Summary:PDF Full Text Request
Drug residues in food are potentially harmful to the consumers. As the basis of sample detection and market surveillance, simple, rapid and robust analytical methods for drug residues determination in food matrix are therefore very necessary. In this study, liquid chromatography (LC) or liquid chromatography tandem mass spectrometry (LC-MS/MS) methods were developed for the detection of multi-antifungal agent in food samples.1. An LC-MS/MS method was presented for the simultaneous quantification of 10 antifungal drugs (voriconazole, griseofulvin, clotrimazole, bifonazole, econazole, ketoconazole, itraconazole, miconazole, terconazole and fluconazole) in chicken liver and muscle. Homogenized tissue samples were extracted with acetonitrile and followed by freezing-delipidation. An Acquity UPLCTM BEH C18 column was used to separate the analytes, coupled with tandem MS using an electrospray ionization source. Overall average recoveries at three levels ranged over 68-120% with relative standard deviation (RSD) from5% to 23% (n=6). The LOQ of these compounds in two different matrices was 0.50-3.0μg·kg-1.2. Determination of natamycin in 6 kinds of jam by liquid chromatography tandem mass spectrometry was developed in this paper. After adding NaCl, jam samples were extracted by acetone and separated on BEH C18 column, coupled with tandem MS. The recovery at three spiked levels was 80-113% with the relative standard deviation less than 20% (n=5). The LOQ of natamycin in jam was 0.5-1.0μg·kg-1.3. Determination method of 3 kinds of polyenes antifungal agents in bread, pastries and yogurt was established. Samples were ultrasonic extracted by methanol with Na2EDTA being added, then the supernatant was diluted with water and purified by C18 cartridges. Target drugs were separated on BEH C18 column and assayed by LC-UV or LC-MS/MS. For LC-UV method, the recoveries at three spiked levels were 79-103% with acceptable coefficients of variation (2-10%, n=5), and the LOQ was 0.05-1.0 mg·kg-1. As well as the LC-MS/MS analysis, the recoveries was 75-113% with RSD less than 22%(n=5) and the LOQ was 0.5-5.0μg·kg-1.
Keywords/Search Tags:HPLC-MS/MS, HPLC, residues, antifungal agents
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