分析测试学报2012，Vol.31Issue(11)：1416-1420,5.DOI:10.3969/j.issn.1004-4957.2012.11.013
动物组织中硝呋索尔代谢物残留量的液相色谱串联质谱法测定
Determination of Metabolite Residue of Nifursol in Animal Tissue by High Performance Liquid Chromatography-Tandem Mass Spectrometry
赵凤娟 1肖陈贵 1岳振峰 1张毅 1欧阳姗 1康海宁 1韩瑞阳1
作者信息
- 1. 深圳出入境检验检疫局食品检验检疫技术中心,广东深圳518045
- 折叠
摘要
Abstract
A high performance liquid chromatography tandem mass spectrometric ( HPLC - MS/MS) method was developed for the determination of nifursol metabolite 3, 5-dinitrosalicylic acid hydrazide (DNSAH) residue in animal tissues. The sample was extracted with ethyl acetate after hydrolysised and derivatized, then cleaned up by n-hexane. The condensed sample solution was separated on a reversed-phase column of Thermo Hypersil Gold C18(100 mm ×2. 1 mm i. d. , 1. 9 μm)by gradient elution with methanol - water as mobile phase at a flow rate of 0. 3 mL/min. The quantitation detection was performed by HPLC -tandem MS using multiple reaction monitoring ( MRM) under negative ion electrospray ionization. The calibration curve of DNSAH was linear in the range of 0. 5 -5. 0 μg/ kg. The limit of quantitation was 0. 5 |xg/kg. The recoveries at three spiked levels were between 91% and 103% with RSDs(n =6) of 3. 7% -13.6%. The method was sensitive and accurate, and could meet the requirements of the domestic and international legislations. Therefore, the method was suitable for the determination and confirmation of residue of nifursol metabolite in animal tissues.关键词
液相色谱-串联质谱/硝呋索尔/动物组织/残留Key words
liquid chromatography - tandem mass spectrometry ( LC - MS/MS ) / nifursol/ animal tissue/ residue分类
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赵凤娟,肖陈贵,岳振峰,张毅,欧阳姗,康海宁,韩瑞阳..动物组织中硝呋索尔代谢物残留量的液相色谱串联质谱法测定[J].分析测试学报,2012,31(11):1416-1420,5.
