| Veterinary medicine are commonly used antimicrobial agents, which has the features of broad-spectrum, highly efficient, and has been used widely in modern farming industry.. And its widely application in the aquaculture industry, their resdues become a prominent problem, and caused widespread concern, and the residues detetion technology has also been developed rapidly. In this paper, ultra-high performance liquid chromatography - tandem mass spectrometry method for simultaneous determination of several veterinary medicine residues in eel had been developed and satisfactory results had been obtained.This article consists of four parts. In Part I, the characters of veterinary medicine had been introduced, General extraction and detection techniques for animal origin had been summarized. And the purpose of this study had been introduced.In Part two, the detail of the experiment had been described, a high performance liquid chromatography - tandem mass spectrometry method for simultaneous determination of fifteen quinolones residues in eel had been established. Samples were extracted with acetonitrile, chromatographic pure defatted with hexane, and then backward through 0.22um pore-like membrane purification, waters Acquity UPLC BEH C18 column (55mm×2.1mm,1.7μm) had been used, the chromatography pure acetonitrile and 10mmol/L ammonium acetate buffer was used as the mobile phase, gradient elution approach had been chosen and MS has been chosen as a detector, MRM positive ion mode scanning has been chosen as the scan mode. The standard sample, recovery of samples, blank samples and four unknown samples had been detected with satisfied results.In Part three, malachite green, crystal violet, acetonitrile had been applied for rapid detection kit and methyl cyanide for sample extraction, malachite green special column for solid phase extraction purification, and triple quadrupole UPLC-MS/MS had been applied for determination. In the 0.5 μg/kg standard adding conditions, malachite green, leucomalachite green, crystal violet and leucocrystal violet, the recoveries were 123.%,109.6%,126.4%,106.2%, respectively. The actual detection methods had been verified by testing a large number of eel samples The pre-treatment process is efficient, and the detection results were accurated., the detection process were faster and more suitable for aquatic food needs of business-to-sample test. Objects can not only measure the accurate quantification of treatment, but also qualitatively confirmed the analytes for the monitoring of drug residues and provide strong technical support for drug residues inspection.Since nitro furan quickly degradated in the animal body and its products, and the protein binding metabolites of nitro furan degradation may be retained for a long time in animal food organization, therefore detection of nitro furan drugs is importanted. In Part four, Many methods such as high efficiency liquid chromatography (HPLC), Liquid chromatographic tandem mass spectrometry(LC-MS/MS), spectrophotometry, ELISA, and UPLC had been applied to detect nitro furan. HPLC method has the merits of hig efficiency, high sensitivity and high automation; UPLC instruments need rigourly sample purification; ELISA method can easily cause false positiver; Spectrophotometry method has low accuracy and sensitivity. LC - MS/MS owns the feature of wider analysis range, high separate ability, reliable qualitative analysis, low detection limit, short analysis time and a high degree of automation, which is very suitable for nitro furan drugs tests; Therefore, liquid chromatographic tandem mass spectrometry had been applied to detect nitrofuran in eel samples in this study. |
PDF Full Text Request