摘要
采用同位素内标稀释技术建立了动物性食品中呋喃唑酮、呋喃它酮、呋喃西林、呋喃妥英代谢物的测定方法,在酸性条件下水解,2-邻硝基苯甲醛溶液(2-NBA)进行衍生化,乙酸乙酯提取,固相萃取柱OasisHLB富集净化,三级四极串联电喷雾质谱正离子模式测定,同位素内标定量。本方法检出限0.1μg/kg,加标回收率65.3%～83.7%,相对标准偏差3.1%～12.6%。该方法灵敏度高、重现性好、定性准确可靠。通过对实际样品的检测,证明可用于动物源性食品中四种硝基呋喃代谢物残留的测定。
A liquid chromatography -tandem mass spectrometry （LC - MS/MS） method based on isotope dilution has been developed for determination of four nitrofuran metatolites residues in food originated from animals. The procedure includes an acid-catalyzed release of protein-bound nitrofuran metabolites, and derivatization with 2-nitrobenzaldehyde. Sample extraction are used ethyl acetate and clean-up was performed by solid-phase extraction（SPE）, then detected by positive electrospray ionization（ESI）LC - MS/MS. Reliable quantity is obtained by using internal standard. The minimum quantification limits are 0.1 μg/kg Average recoveries are ranges from 65.3%- 83.7%. The relative standard deviation are in the range of 3.1%-12.6% Validation of the method was conducted for the analysis of residues in pork. False positive SEM is discussed. The method is sensitive and suitable for routine quality control operations.
出处
《现代畜牧兽医》
2008年第1期47-50,共4页
Modern Journal of Animal Husbandry and Veterinary Medicine
关键词
硝基呋喃类代谢物
液质联用
残留
Nitrofuran metatolites
Liquid chromatography mass spectrometry Residues
