高效液相色谱法与串联质谱联用法应用于香肠中硝基呋喃代谢物的测定.试样在稀盐酸溶液中同时加入一定量的衍生试剂邻硝基苯甲醛后,在37 ℃放置过夜使其中与蛋白质结合的硝基呋喃代谢物水解并衍生化.将此溶液的酸度调节至pH 7.0~7.5后,以3 000 r·min-1的转速离心10 min，分出上层清液，用乙酸乙酯萃取.所得萃取液用作HPLC-MS/MS测定.在电喷雾正离子条件下，用多离子反应监测模式，以外标法对萃取液中对经衍生化后的各硝基呋喃代谢物进行定量.在0.5~10 μg·kg-1范围内进行标准加入回收试验，4种硝基呋喃代谢物的回收率在77.3%~90.7%之间，测定值的相对标准偏差小于9%.测得方法的检出限(S/N=3)为:0.10 μg·kg-1对呋喃唑酮、呋喃它酮及呋喃西林的代谢物和0.20 μg·kg-1对呋喃妥因代谢物.

High performance liquid chromatography in hyphenation with tandem mass spectrometry (LC-MS/MS) was applied to the determination of matabolites of nitrofuransin ausage.Protein combined metabolites in the sample were hydrolyzed and derivatized with 2-nitrobenzaldehyde overnight at 37 ℃ in dil.HCl solution.Acidity of the solution was adjusted to pH 7.0-7.5,and centrifuged at 3 000 r·min-1 for 10 min.The supernatant layer was separated and extracted with ethyl acetate.Derivatized products of metabolites of nitrofurans were then determined by HPLC-MS/MS under the condition of electrospray ionization in positive mode (ESI+) using multi-ionic reaction monitoring.Method of external standard was used in the determination.Recovery tests were made by addition of standards in the range of 0.5-10 μg·kg-1,and results obtained were ranging from 77.3% to 90.7% with values of RSD′s less than 9%.Detection limits (S/N=3) of the method were found to be 0.10 μg·kg-1 for metabolites of 3-amino-2-oxazolidinone (AOZ),5-methylmorpholino-3-amino-2-oxazolidinone (MAOZ) and semicarbazide (SC),and 0.20 μg·kg-1 for 1-amino-hydantoin (AHD).