分析测试学报2009，Vol.28Issue(7)：784-788,793,6.DOI:10.3969/j.issn.1004-4957.2009.07.006
UPLC-MS/MS法对动物源性食品中12种大环内酯类抗生素残留的测定
Determination of 12 Macrolide Antibiotics Residues in Products of Animal Origin by Ultra Performance Liquid Chromatography Coupled with Tandem Mass Spectrometry
摘要
Abstract
An ultra performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS) method was developed for simultaneous determination of 12 macrolide antibiotics,e.g.lincomycin(LIN),azithromycin(AZI),spiramycin(SPM),tilmicosin(TIL),oleandomycin(OLD),josamycin(JOS),tylosin(TYL),kitasamycin(KIT),roxithromycin(ROM),clarithromycin(CLA),mydecamycin(MYD),erythromycin(ERM) in products of animal origin.Homogenized samples were extracted twice with acetonitrile.The extracts were partitioned with hexane to remove the animal fats and dehydrated with sodium sulphate anhydrous.The extract layer was evaporated to dryness and the residue was redissolved in methanol.Identification of 12 macrolide antibiotic was achieved by electrospray ionization tandem mass spectrometry in positive mode using multiple reaction monitoring(MRM) and quantification analysis was performed with matrix-matched standard calibration.The results indicated that,under the optimal conditions,the calibration curves showed good linearity for 12 macrolide antibiotics over the concentration range of 5-100 μg/kg.Detection limits were 5.0 μg/kg and quantification limits were 10 μg/kg for all the analytes.The mean recoveries varied from 60% to 117% at three spiked levels of 10,25,50 μg/kg.The RSDs were less than 20%.This method is sensitive and reproducible,and it meets the requirements of the domestic and international legislation.Therefore,it is suitable for the routinely determination of 12 macrolide antibiotics residues in products of animal origin.关键词
大环内酯抗生素/超高效液相色谱-串联质谱/动物源性食品Key words
macrolide antibiotic/ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)/products of animal origin分类
化学化工引用本文复制引用
王凤美,陈军辉,林黎明,汤志旭..UPLC-MS/MS法对动物源性食品中12种大环内酯类抗生素残留的测定[J].分析测试学报,2009,28(7):784-788,793,6.基金项目
山东出入境检验检疫局科研基金资助项目(SK200621) （SK200621）
