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基于UPLC-MS/MS同时测定猪粪便中5种兽药残留量的研究
顾欣
0
(上海市动物疫病预防控制中心)
摘要:
本文建立了同时测定猪粪便中二甲氧苄啶、磺胺对甲氧嘧啶、恩诺沙星、金霉素、泰乐菌素5种兽药残留量的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。样品经McIlvaine-Na2EDTA缓冲溶液提取,C18粉吸附杂质,HLB固相萃取小柱净化,浓缩富集后用0.1%甲酸甲醇溶液复溶,过滤上机,基质液外标法定量。结果显示,5种兽药在10~500 μg/kg的质量浓度范围内线性良好,在添加浓度50~500 μg/kg,平均回收率为53%~85%,RSD为1.87%~18.81%。该方法具有较好的准确度与精密度,能快捷地测定猪粪便中5种兽药。
关键词:  超高效液相色谱-串联质谱  兽药残留  猪粪便
DOI:
投稿时间:2015-08-03修订日期:2015-09-21
基金项目:上海市科技兴农重点攻关项目(沪农科攻字(2014)第3-3号),公益性行业(农业)科研专项(项目编号:201203023)
Simultaneous determination of five veterinary drug residues in swine manure by ultra-performance liquid chromatography-tandem mass spectrometry
顾欣
(Shanghai Animal Disease Control Center)
Abstract:
A method for simultaneously detecting Diaveridine, Sulfameter, Enrofloxacin, Chlorotetracycline and Tylosin in swine manure by ultra-performance liquid chromatography-tandem mass spectrometry was developed. After having been extracted with McIlvaine-Na2EDTA buffer solution, the sample was purified and concentrated by C18 power and HLB Solid phase extraction column. The residue was dissolved by 0.1% formic acid/methanol (85/15).The results showed that five veterinary drugs were determined with a fine linear relationship from 10 to 500 μg/kg. The recoveries of five veterinary drugs spiked with 50~500 g/kg in swine manure were from 53%~85%with RSDs ranging from 1.87% to 18.81%. As a result, the method is seized of high accuracy as well as sensitivity for a rapid determination of five veterinary drugs in swine manure.
Key words:  ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)  veterinary drug residues  swine manure

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