液相色谱-电喷雾质谱联用检测蜂蜜中四种硝基呋喃类代谢物

Determination of four metabolites of nitrofuran antibacterial drugs in honey by liquid chromatograph-electrospray ionization-mass spectrometry

介绍了高效液相色谱-电喷雾多级质谱(LC/MSn)同时快速、准确测定蜂蜜中呋喃西林、呋喃唑酮、呋喃它酮和呋喃妥英4种硝基呋喃类抗生素代谢物.硝基呋喃类代谢物在酸性条件下经过邻硝基苯甲醛衍生化,液相萃取后经色谱分离,利用二级质谱进行定性和定量.加标样品平均回收率达到64%～79%,定量下限(LOQ)为0.1～1 μg*kg-1,检测限(LOD)达到0.05～0.5 μg*kg-1.该方法测定结果满足欧盟(EU)对进口动物源性食品中硝基呋喃类抗生素的残留要求.

A liquid chromatography-electrospray ionization multi-stage mass spectrometry (LC-ESI-Msn) method was developed for the simultaneous determination of the metabolites of four nitrofuran antibiotics in honey. Sample clean-up and analyte enrichment were performed by Liquid-Liquid extraction with ethyl acetate following combined hydrolysis and derivatization with 2-nitrobenzaldehyde (2-NBA). Limit of detection (LOD) of 0.05~0.5 μg kg -1 and limit of quantitation (LOQ) of 0.1~1 μg kg -1 were achieved using electrospray ionization (ESI) in positive mode. The recovery rates were in the range of 64%～82%. All of the analytical results conformed to the guidelines of European Union.