高效液相色谱-串联质谱法测定动物源性食品中硝基呋喃类代谢物残留量

依次用甲醇、乙醇和乙醚溶剂提取，使动物源性样品中呋喃唑酮、呋喃西林、呋喃它酮、呋喃妥因等4种硝基呋喃类游离态代谢物进入提取液，而结合态代谢物保留在残渣中。在酸性条件下用2-硝基苯甲醛分别衍生游离态和结合态代谢物，经乙酸乙酯提取浓缩后，用液相色谱-四极杆串联质谱仪定性，用同位素内标法定量。检出限均为0．3μg/kg。在0．3、1．0和5．0μg/kg3个浓度水平上进行加标回收试验，回收率为85．2％～112．5％，相对标准偏差均不大于6．3％(n=6)。

DETERMINATION OF THE NITROFURAN METABOLITE RESIDUES IN ANIMAL ORIGIN FOOD BY HPLC -TANDEM MASS SPECTROMETRY

Having been extracted by methanol, ethanol and ethyl ether in turns, free residues of four nitrofuran metabolites(furazolidone, furaltadone, nitrofurazone and nitrofurantoin) in animal tissue entered extracted liquid, meanwhile bounded residues were kept in the leavings. Free residues and bound residues were derived separately with 2-nitrobenzaldehyde in acid medium. After extracted by ethyl acetate and concentrated, identification and quantification of analyte was performed by HPLC-triple quadrupole tandem MS using isotope as the internal standard. The limits of quantification were 0.3 g/kg. The recoveries were 85.2%~112.5% at three levels of 0.3, 1.0 and 5.0 g/kg, the relative standard deviations were no more than 6.3%(n=6).