质谱学报2013，Vol.34Issue(2)：82-87,6.DOI:10.7538/zpxb.2013.34.02.0082
高效液相色谱-串联质谱法检测动物源食品中硝呋索尔代谢物残留
Determination of the Metabolite of Nifursol in Animal Origin Food by HPLC-MS/MS
摘要
Abstract
A method of liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) was developed for the determination of 3,5-dinitrosalicylic acid hydrazine (DN-SH), which was the metabolite of nifursol antibiotic in animal origin food. The samples were hydrolyzed with 0. 1 mol/L HC1, and derivatised with 2-nitrobenzaldehyde at 37 ℃ for 16 h. The derivative solutions were adjusted to pH 7. 0-7. 5, and extracted by ethyl acetate. The analyte was detected by tandem mass spectrometry with electrospray ionizationsource by MRM mode. There is good linear correlation between the peak areas and concentrations of DNSH(the calibration coefficient is 0. 999 5), the dynamic linear range is 0. 5-10 μg/kg. The limit of detection (S/N = 3) is 0. 5 μg/kg. The recoveries of DNSH at four spiked levels of 0. 5, 1.0, 2. 0, 4. 0 μg/kg range from 63. 4% to 109. 5% (n = 6) and the RSDs are between 2. 0% and 11. 9% (n = 6). It is proved to be fast and effective for simultaneously qualitative and quantitative inspection of the metabolite of nifursol antibiotic in animal origin food.关键词
硝呋索尔/3,5-二硝基水杨酸肼/动物源食品/液相色谱-串联质谱法Key words
nifursol/ 3,5-dinitrosalicylic acid hydrazine (DNSH)/ animal origin food/ liquid chromatography-triple quadrupole tandem mass spectrometry (LC-MS/MS)分类
化学化工引用本文复制引用
黄帆,王传现,张缙,盛永刚,王敏,韩丽,李晓虹,徐敦明,刘茜..高效液相色谱-串联质谱法检测动物源食品中硝呋索尔代谢物残留[J].质谱学报,2013,34(2):82-87,6.基金项目
上海市科委工程中心建设项目(11DZ2280300) （11DZ2280300）
上海市科委重点科技攻关项目(10391901800) （10391901800）
上海市科委长三角联合攻关项目(11495810200)资助 （11495810200）
